反应详情

温度

20 °C

A solution of chlorotrimethylsilane (200 mL) in methanol (300 mL) was treated with 2-chloro-5-fluoro-4-methyl-3-nitrobenzoic acid (Preparation 1c, 65.5 g) portionwise under nitrogen. The resulting solution was stirred at 20° C. for 16 h. Further chlorotrimethylsilane (100 mL) was added and the reaction heated at 50° C. for 6 h. The reaction mixture was evaporated to afford crude product which was diluted with water and extracted with ethyl acetate (300 mL). The organic extract was dried (MgSO4), filtered and evaporated to afford the subtitle compound (53.4 g).

1. temperaturethe reaction heated at 50° C. for 6 h
2. customThe reaction mixture was evaporated
3. customto afford crude product which
4. extractionextracted with ethyl acetate (300 mL)
5. extractionThe organic extract
6. dry with materialwas dried (MgSO4)
7. filtrationfiltered
8. customevaporated