Brief introduction 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

Acetylferrocene was synthesizedaccording to previously reported procedures [49]. Briefly, 85% phosphoric acid (4?mL) was slowly added to a stirred solution of ferrocene (4.0?g, 21.5?mmol) and acetic anhydride (13.3?mL, 140.0?mmol). The mixture was heated in a water bath maintained at 50?C for 10?min and then cooled in ice. Water (25?mL) was added to the mixture, that was then neutralized with NaHCO3 until the end of CO2 formation. CH2Cl2 (50?mL) was added and the orange organic layer was separated and retained in the dark, whereas the brown-coloured aqueous layer washed with a further 20?mL of CH2Cl2. The combined organic fractions were washed twice with water and then dried with anhydrous magnesium sulfate. Crude acetyl ferrocene, obtained removing the solvent under reduced pressure, was purified by silica gel column chromatography using a 95/5 mixture of petroleum ether/ethyl acetate as starting eluent to first separate the unreacted ferrocene. Once the ferrocene was eluted, the eluent was replaced by 100% ethyl acetate to collect acetyl ferrocene, that was then obtained by removing the solvent on a rotary evaporator.

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

Reference£º
Article; Paucar, Rocio; Martin-Escolano, Ruben; Moreno-Viguri, Elsa; Cirauqui, Nuria; Rodrigues, Carlos Rangel; Marin, Clotilde; Sanchez-Moreno, Manuel; Perez-Silanes, Silvia; Ravera, Mauro; Gabano, Elisabetta; European Journal of Medicinal Chemistry; vol. 163; (2019); p. 569 – 582;,
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.

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.

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.

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

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

 

Brief introduction 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

To a solution of anhydrous AlCl3 (1.6 g, 12.0 mmol) in CH2Cl2 (20 mL) acetyl chloride (935.8 mg, 12.0 mmol) in CH2Cl2 (10 mL) was added at -5 C. The above mixture was dropwisely added to the solution of ferrocene (1.86 g, 10 mmol) and CH2Cl2 (20 mL) at 0 C and the solution color changed from orange to bluish violet. Then the reaction mixture was warmed to room temperature and stood for 2 h. The mixture was poured to ice-water and the organic phase was successively washed with 1N HCl solution, water and 5% aqueous Na2CO3. The organic layer was dried over anhydrous magnesium sulfate, filtered and the filtrate was concentrated under reduce pressure to give a crude product. The crude product was purified by recrystallization from petroleum ether (60-90 C) to give compound 7a (77.1%).

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

Reference£º
Article; Chen, Peiqi; Liu, Chunjuan; Hu, Jianfeng; Zhang, Hao; Sun, Ranfeng; Journal of Organometallic Chemistry; vol. 854; (2018); p. 113 – 121;,
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

 

Downstream synthetic route of 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) Synthesis of ferrocene formaldehyde: under the protection of the helium gas, in the ice-bath cooling, constant pressure in the funnel 14.6 g (0.2 muM) DMF dimethyl formamide in 10 minutes into the 18.6 g (0.1 muM) ferrocene 75 ml dry chloroform solution; then, 30.6 g (0.2 muM) phosphorus oxychloride in a half-hour in dripped into the reaction bottle, the completion of the dropping, the oil bath temperature to 60 C, heating and stirring 20 hr, the oil bath temperature is still lower than the 60 C; the completion of the reaction, the reaction mixture is poured into ice water, the solid is most unreacted ferrocene, filtering to filter the solid insoluble matter, the filtrate magnesium carbonate powder carefully neutralized, then circulating extraction device repeatedly extraction reaction mixture, all of the extracts combined, water washing, the organic layer using sodium carbonate drying, to remove the solvent to obtain the crude product 18.21 g, dichloromethane is used for – hexane recrystallize to get red brown crystal 15.0 g, yield of 72.4%.

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

Reference£º
Patent; Shandong Yuangen Petrochemical Co., Ltd.; Qiao Liang; Yuan Junzhou; Song Laigong; He Jingsong; Liu Shanshan; (7 pag.)CN104710482; (2018); B;,
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

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. Quickly pour the reaction solution into crushed ice, adjust the pH to 6-7 with sodium bicarbonate solids, and filter to obtain acetylBasic ferrocene crude;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 Ferrocene 7611, airon-catalyst compound, is more and more widely used in various.

Reference£º
Patent; Suzhou Tianyun Metal Materials Co., Ltd.; Wang Ming; (5 pag.)CN107488200; (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.

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

The mixture of ferrocene (2.79 g, 15 mmol), DMF (2.19 g, 30 mmol) and chloroform (11 mL) was stirred at 0 C under N2 atmosphere. Phosphorus oxychloroide (4.59 g, 30 mmol) was added slowly over a period of 30 min at 0 C and stirred at the temperature range of 55-60 C for 24 h until the reaction was completed. The mixture was poured into ice-water (100 mL) and neutralized with 5% aqueous Na2CO3 accompanying the precipitate formation. The precipitate was filtered off and the filtrate was extracted with 100 mL of toluene. Then the organic phase was washed three times with water, dried over anhydrous magnesium sulfate, filtered and the filtrate was concentrated under reduced pressure to give a crude product. The crude product was purified by column chromatography on silica gel to give compound 8a as a crimson solid (75.7%).

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

Reference£º
Article; Chen, Peiqi; Liu, Chunjuan; Hu, Jianfeng; Zhang, Hao; Sun, Ranfeng; Journal of Organometallic Chemistry; vol. 854; (2018); p. 113 – 121;,
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.

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.

Step (1): Under a nitrogen system,10 g (53.8 mmol) of ferrocene was first dissolved in 50 mL of anhydrous n-hexane,Further, 18.1 mL (84.5 mmol) of tetramethylethylenediamine (TMEDA) was added,And 48.0 mL of n-hexane solution of 2.5 M n-butyllithium (n-BuLi) was slowly added dropwise at 0 C,And stirred at 25 C. After stirring for 12 hours,Remove the solvent first,And the resulting pale orange yellow complex was added to 200 mL of ethyl ether and the mixture was stirred and cooled to -78 C,Slowly drop the iodine ether solution (19.0 g I2 / 350 mL)Ether)After slowly warming to 25 C and stirring for 1 hour,The reaction was poured into 100 mL,5 wt% aqueous solution of ferric chloride (FeCl3)And then extracted with 200 mL of ether,The resulting organic layer was washed 10 times with 5 wt% of ferric chloride (FeCl3) aqueous solution (100 mL)And then washing the organic layer with water to the water layer is no longer discolored,To remove water with anhydrous magnesium sulfate (MgSO4) and remove the solvent,To obtain a mixture of compound a and compound b in a dark brown and liquid form(The molar ratio of compounds a and b is 1: 1; compounds a and b are shown in reaction I). Step (2):2.5 g (6.67 mol) of the mixture obtained in step (1)128 mg (0.67 mmol) of cuprous iodide (CuI),107 mg (0.67 mmol) of ferric chloride (FeCl3),540 mg (13.3 mmol) of sodium hydroxide,30 mL of aqueous ammonia (15 M) and 30 mL of ethanol (EtOH) were placed in a 150 mL autoclave,And then reacted at 90 C for 12 hours and lowered to 25 C,200 mL of diethyl ether was poured and washed three times with 150 mL of a 1.0 M aqueous solution of sodium hydroxide,After removing water with anhydrous magnesium sulfate and removing the solvent,To obtain a crude orange-brown product.At last,The crude orange-brown product was purified by column chromatography using 1: 2 (v / v ethyl acetate and n-hexane)To obtain a yellowish amine ferrocene solid (yield 48%).

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

Reference£º
Patent; Zheng, Jianhong; Lai, Zhenchang; Zhang, Yuwei; Liao, Chunyi; Huang, Minjie; (31 pag.)CN106317129; (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