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;,
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