Analyzing the synthesis route of 102-54-5

The synthetic route of 102-54-5 has been constantly updated, and we look forward to future research findings.

With the rapid development and complex challenges of chemical substances, new drug synthesis pathways are usually the most effective.102-54-5,Ferrocene,as a common compound, the synthetic route is as follows.,102-54-5

General procedure: A solution of acid chloride (63mmol) in 30ml dry dichloromethane was added to a suspension of anhydrous aluminum chloride (8.41g, 63mmol) in 30ml dry dichloromethane and the mixture was stirred at 5C for 1h under Argon. The solution of aluminum chloride: acid chloride complex was added dropwise over 30min to a solution of ferrocene (11.16g, 60mmol) in 100ml dry dichloromethane at 0C. The reaction mixture was warmed to room temperature and stirred for 16h. A solution of NaBH4 (2.38g, 63mmol) in 25ml diglyme was added dropwise to the purple reaction mixture at-5C. An orange solution was formed and stirred at 0C for 1h. The mixture was then hydrolyzed with addition of 20ml water while maintaining its temperature at less than or equal to 10C. The mixture was allowed to separate by settling and the organic phase was then withdrawn. The aqueous phase was extracted with 3 times 30ml of dichloromethane and then all the organic phases are combined. Combined organic layer was washed with 50ml of brine and then dichloromethane was distilled under atmospheric pressure. The diglyme and the residual ferrocene which was found to be entrained by the diglyme were then distilled at reduced pressure approximately 20mm Hg and a column head temperature of 85-95C. The alkylferrocene derivatives were distilled at a more reduced pressure, less than 5mm Hg.

The synthetic route of 102-54-5 has been constantly updated, and we look forward to future research findings.

Reference£º
Article; Teimuri-Mofrad, Reza; Safa, Kazem D.; Rahimpour, Keshvar; Journal of Organometallic Chemistry; vol. 758; (2014); p. 36 – 44;,
Iron Catalysis in Organic Synthesis | Chemical Reviews
Iron Catalysis in Organic Synthesis: A Critical Assessment of What It Takes To Make This Base Metal a Multitasking Champion

 

Simple exploration of 102-54-5

102-54-5 Ferrocene 7611, airon-catalyst compound, is more and more widely used in various.

102-54-5, Ferrocene is a iron-catalyst compound, ?involved in a variety of chemical synthesis. Rlated chemical reaction is continuously updated,102-54-5

Add 100ml of dichloromethane to the reaction flask, add 20g of ferrocene, then add 16g of ZnCl2, then add 10g of acetyl chloride to stir at room temperature, control the reaction, after the reaction is over, add the reaction solution In a 5% aqueous solution of hydrochloric acid, the liquid phase was separated, and the organic phase was washed three times with water, and the organic phase was separated. The organic phase was dried and concentrated to give 22 g of acetyl ferrocene in a yield of 90%.

102-54-5 Ferrocene 7611, airon-catalyst compound, is more and more widely used in various.

Reference£º
Patent; Nanjing Faen Chemical Co., Ltd.; Wang Kunpeng; Han Yuelin; (5 pag.)CN108409801; (2018); A;,
Iron Catalysis in Organic Synthesis | Chemical Reviews
Iron Catalysis in Organic Synthesis: A Critical Assessment of What It Takes To Make This Base Metal a Multitasking Champion

 

New learning discoveries about 102-54-5

As the paragraph descriping shows that 102-54-5 is playing an increasingly important role.

With the rapid development and complex challenges of chemical substances, new drug synthesis pathways are usually the most effective.102-54-5,Ferrocene,as a common compound, the synthetic route is as follows.

1. Mix acetic anhydride and phosphoric acid and stir at room temperature for 15 minutes;2, adding ferrocene solids, heated to 40 C for 1 hour;3. Raise the temperature to 50 C and react until the ferrocene reaction is complete;4. The reaction solution is rapidly poured into crushed ice, and the pH is adjusted to 6 to 7 with sodium bicarbonate solids, and the crude acetylferrocene is obtained by filtration.5. Pure acetyl ferrocene is obtained by recrystallization from petroleum ether.In this example, acetic anhydride: phosphoric acid: ferrocene solids = 3:1:0.5.By elemental analysis tests, the product was confirmed to be acetylferrocene.The yield is above 95%.The reaction conditions for the synthesis of acetylferrocene are mild, the temperature is easy to control, and the preparation yield is high., 102-54-5

As the paragraph descriping shows that 102-54-5 is playing an increasingly important role.

Reference£º
Patent; Suzhou Tianyun Metal Materials Co., Ltd.; Wang Ming; (5 pag.)CN107488199; (2017); A;,
Iron Catalysis in Organic Synthesis | Chemical Reviews
Iron Catalysis in Organic Synthesis: A Critical Assessment of What It Takes To Make This Base Metal a Multitasking Champion

 

Some tips on 102-54-5

102-54-5 Ferrocene 7611, airon-catalyst compound, is more and more widely used in various.

With the rapid development and complex challenges of chemical substances, new drug synthesis pathways are usually the most effective.102-54-5,Ferrocene,as a common compound, the synthetic route is as follows.,102-54-5

In a three-necked flask equipped with a thermometer, 3.72 g (0.02 mol) of ferrocene and 18.86 mL (0.2 mol) of acetic anhydride were added 3.3 mL (0.06 mol) of phosphoric acid was added dropwise with stirring. The temperature was controlled at 55-60C and the TLC point plate was followed to complete conversion of ferrocene. After adding saturated Na2CO3 solution to neutralize to pH=7, the mixture was extracted with methylene chloride (30 mL x 3) and the combined organic phases were washed with water and dried over anhydrous magnesium sulfate. Column separation. 3.86 g of pure acetylferrocene was obtained. Yield : 85%.

102-54-5 Ferrocene 7611, airon-catalyst compound, is more and more widely used in various.

Reference£º
Patent; Zhengzhou University of Light Industry; Yu Shuyan; Zhang Tongyan; Wang Ruijuan; Yin Zhigang; Yang Xuzhao; Lan Hongbing; (13 pag.)CN107383112; (2017); A;,
Iron Catalysis in Organic Synthesis | Chemical Reviews
Iron Catalysis in Organic Synthesis: A Critical Assessment of What It Takes To Make This Base Metal a Multitasking Champion

 

New learning discoveries about 102-54-5

As the paragraph descriping shows that 102-54-5 is playing an increasingly important role.

With the rapid development and complex challenges of chemical substances, new drug synthesis pathways are usually the most effective.102-54-5,Ferrocene,as a common compound, the synthetic route is as follows.,102-54-5

A 250 mL round bottom reaction flask was charged sequentially with 1.46 g of aluminum trichloride (11 mmol) and 20 mL of dichloroethane,Under ice-water cooling, 0.8 mL of acetyl chloride (11 mmol)Continue stirring until almost dissolved aluminum trichloride.In another 250 mL round bottom reaction flask,A solution of 1.86 g (ie 10 mmol) of ferrocene in dichloroethane was added,Under ice-cooling, the acetyl chloride-aluminum trichloride complex solution prepared above was dropped,Stirring to complete the reaction at room temperature (monitored by thin layer chromatography) takes about 2 hours.The reaction was poured into ice water,Separate the organic phase,Followed by water,5% sodium carbonate solution and water,Drying over anhydrous sodium sulfate.The solvent was removed under reduced pressure,A red oil was obtained,Recrystallization to give orange crystals of acetyl ferrocene,Yield 80%.

As the paragraph descriping shows that 102-54-5 is playing an increasingly important role.

Reference£º
Patent; Inner Mongolia University; Zhang Hao; Ling Li; Hu Jianfeng; Huo Yanhong; (11 pag.)CN107226829; (2017); A;,
Iron Catalysis in Organic Synthesis | Chemical Reviews
Iron Catalysis in Organic Synthesis: A Critical Assessment of What It Takes To Make This Base Metal a Multitasking Champion

 

Analyzing the synthesis route of 102-54-5

With the synthetic route has been constantly updated, we look forward to future research findings about Ferrocene,belong iron-catalyst compound

As a common heterocyclic compound, it belong iron-catalyst compound,Ferrocene,102-54-5,Molecular formula: C10Fe,mainly used in chemical industry, its synthesis route is as follows.,102-54-5

To a solution of ferrocene (1; 5.00 g, 26.87 mmol) in anhydrous CH 2 Cl 2(30 mL), a solution of acetyl chloride (2.01 mL, 28.21 mmol) and AlCl 3(3.94 g, 29.55 mmol) in anhydrous CH 2 Cl 2 (40 mL) was added at 0 C.The reaction temperature was allowed to rise to r.t., and the dark-vio-let solution was stirred for 2 h. The reaction was quenched by addi-tion of ice-cold water (70 mL) at 0 C and the mixture was extractedwith CH 2 Cl 2 (3 ¡Á 70 mL). The collected organic layers were washedwith a solution of Na 2 CO 3 (50 mL), dried over Na 2 SO 4 , filtrated and thesolvent was removed under reduced pressure. Crude product (dark-orange solid) was purified by chromatography on SiO 2 (hexanes/EtOAc = 4:1; R f = 0.3) to afford target product 2.Yield: 4.45 g (73%); orange solid; mp 85-86 C (lit. 20 85-86 C).1 H NMR (300 MHz, CDCl 3 ): delta = 4.78-4.76 (m, 2 H), 4.55-4.42 (m, 2 H),4.20 (s, 5 H), 2.40 (s, 3 H).NMR spectra are in agreement with those of the commercially avail-able product.

With the synthetic route has been constantly updated, we look forward to future research findings about Ferrocene,belong iron-catalyst compound

Reference£º
Article; Plevova, Kristina; Mudrakova, Brigita; ?ebesta, Radovan; Synthesis; vol. 50; 4; (2018); p. 760 – 763;,
Iron Catalysis in Organic Synthesis | Chemical Reviews
Iron Catalysis in Organic Synthesis: A Critical Assessment of What It Takes To Make This Base Metal a Multitasking Champion

 

Analyzing the synthesis route of 102-54-5

With the synthetic route has been constantly updated, we look forward to future research findings about Ferrocene,belong iron-catalyst compound

As a common heterocyclic compound, it belong iron-catalyst compound,Ferrocene,102-54-5,Molecular formula: C10Fe,mainly used in chemical industry, its synthesis route is as follows.,102-54-5

General procedure: An oven-dried vial was charged with anisole 1a (0.75 mmol, 1.0 equiv), acetic anhydride 2a (1.5 mmol, 2.0 equiv) and TFA (0.8 mL). The reaction mixture was stirred at room temperature and monitored by TLC or GC-MS. The reaction typically took 1.5 h to complete. Upon completion, aqueous sodium hydrogen carbonate was added and the aqueous phase was extracted with ethyl acetate (3 x 20 mL). The combined organic layers were dried over Na2SO4 and concentrated. The crude product was purified by silica gel column chromatography to afford ketone product 3a. Alternatively, the product can also be obtained without workup: upon completion, the solvent was removed under reduced pressure and the residue was subjected to silica gel flash column chromatography.

With the synthetic route has been constantly updated, we look forward to future research findings about Ferrocene,belong iron-catalyst compound

Reference£º
Article; Liu, Guangchang; Xu, Bo; Tetrahedron Letters; vol. 59; 10; (2018); p. 869 – 872;,
Iron Catalysis in Organic Synthesis | Chemical Reviews
Iron Catalysis in Organic Synthesis: A Critical Assessment of What It Takes To Make This Base Metal a Multitasking Champion

 

Analyzing the synthesis route of 102-54-5

With the synthetic route has been constantly updated, we look forward to future research findings about Ferrocene,belong iron-catalyst compound

As a common heterocyclic compound, it belong iron-catalyst compound,Ferrocene,102-54-5,Molecular formula: C10Fe,mainly used in chemical industry, its synthesis route is as follows.,102-54-5

General procedure: A solution of acyl chloride (53.76 mmol) in 25 ml drydichloromethane was added to a suspension of anhydrousaluminum chloride (7.7 g, 53.76 mmol) in 25 ml drydichloromethane and the mixturewas stirred at 5 C for 1 hunder argon. The solution of aluminum chloride/acyl chloridecomplexwas added dropwise for 30 min to a solution offerrocene (10 g, 53.76 mmol) in 130ml dry dichloromethaneat 0 C. The reaction mixture was warmed to room temperatureand stirred for 16 h. A solution of NaBH4 (2.29 g,53.76 mmol) in 25 ml diglyme was added dropwise to thepurple reaction mixture at 5 C to form an orange solutionas the result which was stirred for an hour in 0 C. Themixture was hydrolyzed with water while maintaining itstemperature at less than or equal to 10 C. The mixture wasallowed to separate by settling and the organic phase wasthen withdrawn. The aqueous phase was extracted 3 timeswith 30 ml of CH2Cl2 and then all the organic phases werecombined,washed with 50 ml of brine, CH2Cl2was removedand the diglyme and the residual ferrocene which wasfound to be entrained by the diglyme, were distilled atreduced pressure of approximately 20 mm Hg at a columnhead temperature of 85 Ce95 C. The alkylferrocene derivativeswere distilled, at less than 5mmHg. Specific detailsare given for each compound.

With the synthetic route has been constantly updated, we look forward to future research findings about Ferrocene,belong iron-catalyst compound

Reference£º
Article; Teimuri-Mofrad, Reza; Mirzaei, Farzaneh; Abbasi, Hassan; D. Safa, Kazem; Comptes Rendus Chimie; vol. 20; 2; (2017); p. 197 – 205;,
Iron Catalysis in Organic Synthesis | Chemical Reviews
Iron Catalysis in Organic Synthesis: A Critical Assessment of What It Takes To Make This Base Metal a Multitasking Champion

 

Analyzing the synthesis route of 102-54-5

With the synthetic route has been constantly updated, we look forward to future research findings about Ferrocene,belong iron-catalyst compound

As a common heterocyclic compound, it belong iron-catalyst compound,Ferrocene,102-54-5,Molecular formula: C10Fe,mainly used in chemical industry, its synthesis route is as follows.,102-54-5

Under a nitrogen atmosphere, ferrocene (10 g, 53.8 mmol) was dissolved in anhydrous n-hexane (50 ml), followed by adding and mixing with tetramethylethylenediamine (TMEDA, 18.1 ml, 84.5 mmol) A solution of n-butyllithium (n-BuLi) in n-hexane (2.5 M, 48.0 ml) was added slowly dropwise at 0 C., followed by stirring at 25 C. After stirring for 12 hours and removing the solvent, a light orange yellow complex was formed. The complex was added to anhydrous ethyl ether (200 ml), followed by stirring to disperse the complex in anhydrous ethyl ether and lowering the temperature of the dispersion to -78 C. A solution of iodine (19.0 g) in ethyl ether (350 ml) was added to the dispersion slowly dropwise, and the temperature was raised to 25 C. After stirring for a further hour, the reaction was poured into an aqueous ferric chloride (FeCl3) solution (5 wt %, 100 ml), followed by extraction with ethyl ether (200 ml). An organic layer thus obtained was washed ten times with an aqueous ferric chloride (FeCl3) solution (5 wt %, 100 ml) and then was washed with water until the aqueous layer was clear. Thereafter, water was removed using anhydrous MgSO4 and solvent was also removed to obtain a mixture in the form of a blackish brown liquid of compound a and compound b as shown in scheme I in a molar ratio of 1:1. (0037) The obtained mixture (2.5 g, 6.67 mmol), cuprous iodide (CuI, 128 mg, 0.67 mmol), ferric chloride (FeCl3, 107 mg, 0.67 mmol), sodium hydroxide (NaOH, 540 mg, 13.3 mmol), aqueous ammonia (15 M, 30 ml), and ethanol (EtOH, 30 ml) were placed in a high pressure reaction tube of 150 ml. A reaction was conducted at 90 C. for 12 hours. After the temperature of the content in the reaction dropped to 25 C., ethyl ether (200 ml) was added and the content in the reaction tube was washed three times with an aqueous sodium hydroxide solution (1.0 M, 150 ml). Then, water was removed using anhydrous MgSO4 and solvent was also removed to obtain an orange brown crude product, which was purified by column chromatography (eluent: ethyl acetate/n-hexane=1/2 (v/v)) to obtain aminoferrocene compound c shown in Scheme I in the form of a yellowish brown solid (yield: 48%). (0038) 1H NMR (400 MHz, CDCl3) of aminoferrocene compound c: delta 4.08 (s, 5H), 3.97 (t, J=1.6, 2H), 3.82 (t, J=1.6, 2H), 2.58 (br, 2H).

With the synthetic route has been constantly updated, we look forward to future research findings about Ferrocene,belong iron-catalyst compound

Reference£º
Patent; NATIONAL TSING HUA UNIVERSITY; Cheng, Chien-Hong; Lai, Cheng-Chang; Chang, Yu-Wei; Liao, Chuang-Yi; Huang, Min-Jie; (16 pag.)US9356244; (2016); B1;,
Iron Catalysis in Organic Synthesis | Chemical Reviews
Iron Catalysis in Organic Synthesis: A Critical Assessment of What It Takes To Make This Base Metal a Multitasking Champion

 

Analyzing the synthesis route of 102-54-5

The synthetic route of 102-54-5 has been constantly updated, and we look forward to future research findings.

102-54-5, Ferrocene is a iron-catalyst compound, ?involved in a variety of chemical synthesis. Rlated chemical reaction is continuously updated

Ferrocenecarboxaldehyde was prepared from ferrocene according to the literature.10 Phosphorus oxychloride (50mL, 536mmol) was added dropwise to the dimethylformamide (39.0g, 536mmol) at 0C and the resulting mixture was stirred for 30min at this temperature under a nitrogen atmosphere. Next ferrocene (50.0g, 268mmol) in dry chloroform (250mL) was added dropwise to the mixture for 30min at 0C. After completion of the addition, the reaction mixture was kept stirring for 28h with heating at 55-60C on an oil bath, taking care that the temperature did not exceed 60C. The reaction mixture was then cooled to room temperature and neutralized carefully with an aqueous saturated Na2CO3 solution and then extracted repeatedly with the dichloromethane. The combined organic layer was dried over anhydrous Na2SO4, filtered and the solvent was evaporated under reduced pressure. The residue was purified through silica gel column chromatography using hexane/ ethyl acetate mixture (95:05) as eluent to give ferrocenecarboxaldehyde 1 in 55% yield (31.7g) as a reddish brown solid. (mp: 122C, lit.10 123C); IR (KBr, cm-1): 3093, 2837, 2760, 1683, 1447; 1H NMR (400MHz, CDCl3): deltaH 9.95 (s, 1H); 4.80-4.60 (m, 4H), 4.27 (s, 5H); 13C NMR (100MHz, CDCl3): deltaC 193.63, 79.49, 73.33, 69.78; HRMS-ESI (m/z): [M+H]+ Found 215.0157 and calculated 215.0159 for C11H11FeO.

The synthetic route of 102-54-5 has been constantly updated, and we look forward to future research findings.

Reference£º
Article; Achari, Kamsali Murali Mohan; Ramanathan, Chinnasamy Ramaraj; Tetrahedron Asymmetry; vol. 28; 6; (2017); p. 830 – 836;,
Iron Catalysis in Organic Synthesis | Chemical Reviews
Iron Catalysis in Organic Synthesis: A Critical Assessment of What It Takes To Make This Base Metal a Multitasking Champion