反应详情

3.00 g (13.5 mmol) of 3-fluoro-2-methyl-4-trifluoromethylbenzoic acid were initially charged in 50 ml of N,N-dimethylformamide. 1.68 g (purity 60% by weight, 41.9 mmol) of NaH were added a little at a time. Towards the end of the evolution of gas, 1.77 g (purity 95% by weight, 27.0 mmol) of ethanethiol were added dropwise. The mixture was stirred at RT for 2 h and then heated at 80° C. for 10 h. The reaction mixture was cooled and, for workup, poured into ice-water and then acidified with concentrated hydrochloric acid. The product precipitated out and was separated off by filtration. What was isolated were 3.7 g of the pure product.

1. temperatureheated at 80° C. for 10 h
2. temperatureThe reaction mixture was cooled and, for workup
3. customThe product precipitated out
4. customwas separated off by filtration
5. customWhat was isolated