134364-69-5, The chemical industry reduces the impact on the environment during synthesis 134364-69-5, name is 2,3-Difluoroanisole, I believe this compound will play a more active role in future production and life.
The first step: 1000mL four-neck flask, equipped with a thermometer and a condenser tube, under nitrogen protection, put in 2,3-difluoroanisole 57.6g (0.4mol) and 440mL of tetrahydrofuran, start stirring, and lower the temperature to -85 At -75 C, 192 mL (0.48 mol) of n-butyl lithium in hexane solution (2.5 mol / L) was slowly added dropwise. After the addition was completed, the temperature was controlled and stirred for 2.0 hours. After the heat preservation is completed, the temperature is controlled from -85 C to -75 C, and 62.3g (0.6mol) of trimethyl borate is added dropwise. Sample delivery liquid phase detection of 2,3-difluoroanisole raw material residue <0.5%.After the reaction is completed, dehydrolyze tetrahydrofuran under negative pressure until the temperature of the reaction flask reaches 50 C without flow, stop the desolvation, cool to 20-25 C, add 520mL of pure water, control temperature 20-25 C and drop 133.3g (1.0 mol), the dropwise addition was completed and kept stirring for 1.0 hour. 172.8g toluene was added for extraction, the toluene phase was stored separately for use, and the aqueous phase was directly oxidized without further purification. Recover 430.5g of desolvent, send sample to detect water 0.02%, tetrahydrofuran: n-hexane mass ratio is about 4: 1, methanol content is 1.5%, need to remove methanol to apply.
The chemical industry reduces the impact on the environment during synthesis 2,3-Difluoroanisole. I believe this compound will play a more active role in future production and life.
Reference:
Patent; Bengbu Zhong Shi Chemical Co., Ltd.; Xu Jianxiao; Liu Hongqiang; Zhao Shimin; Wei Jiayu; Wang Songsong; Zhu Keming; (7 pag.)CN110922306; (2020); A;,
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