反应详情

1.45 g (6.53 mmol) of 3-fluoro-2-methyl-4-trifluoromethylbenzoic acid were initially charged in 40 ml of DMF. 809 mg (20.2 mmol) of NaH were added a little at a time. After the evolution of gas had ceased, 1.20 g (13.1 mmol) of 2-methoxyethanethiol were added a little at a time. The mixture was stirred at RT for 10 minutes and then heated at 80° C. for 15 h. The reaction mixture was cooled and concentrated under reduced pressure, and for work-up water was added and the mixture was acidified with 1M HCl. The product precipitated and was removed by filtration. The product was then washed with water and n-heptane. What was isolated were 1.7 g of the pure product.

1. temperatureheated at 80° C. for 15 h
2. temperatureThe reaction mixture was cooled
3. concentrationconcentrated under reduced pressure
4. additionfor work-up water was added
5. customThe product precipitated
6. customwas removed by filtration
7. washThe product was then washed with water and n-heptane
8. customWhat was isolated