Related Products of 383-62-0, These common heterocyclic compound, 383-62-0, name is Ethyl 2-chloro-2,2-difluoroacetate, its traditional synthetic route has been very mature, but the traditional synthetic route has various shortcomings, such as complicated route, low yield, poor purity, etc, below Introduce a new synthetic route.
Weigh 2.68g (20mmol) of 4-methyl acetophenone and 13.4ml methyl tert-butyl ether (MTBE), into the reaction flask and stir, 3.70g (23.3mmol) of ethyl difluorochloroacetate was added,A 25% sodium methylate (24 mmol) solution in methanol was added dropwise at room temperature, and the mixture was heated to 45-55 C. during the dropwise addition and stirred for 24 hours.After the reaction was completed, the solvent was concentrated under reduced pressure to give a light yellow solid, which was stirred with 10% diluted hydrochloric acid (v / v) and extracted twice with ethyl acetate. The ethyl acetate layer solution into the reaction flask, add appropriate amount of ethyl acetate and water and stir, add 4.47g (20mmol) p-sulfonamidophenylhydrazine hydrochloride, warmed to 75-85 C, the reaction was stirred for 2 hours, the reaction Completed, room temperature cooling crystallization. Filtration, cake drying 60 C, 60% ethanol (m / m) that was recrystallized, HPLC purity of 99%.
The synthetic route of 383-62-0 has been constantly updated, and we look forward to future research findings.
Reference:
Patent; Nanjing Shenghe Pharmaceutical Co., Ltd.; Wang Yong; Chen Yuqing; Liu Qiang; Liu Yongping; Wang En; (13 pag.)CN104418804; (2017); B;,
Ester – Wikipedia,
Ester – an overview | ScienceDirect Topics