反应详情

With cooling at 10°, 8.5 g of 6,6-difluorohex-5-enoic acid chloride are added to 10.0 g of 4-phenylthioaniline, 6.5 g of triethylamine and 100 mg of 4-N-pyrrolidinopyridine in 250 ml of tetrahydrofuran. The mixture is stirred for 2 hours at room temperature and then concentrated by evaporation in vacuo. The residue is taken up in toluene, the toluene phase is washed with water, dried over sodium sulfate and 90-95% of the amount of toluene is evaporated off in vacuo. While the mixture is still warm, a small amount of hexane is added, which causes the product to crystallise out. The mixture is cooled and filtered, and the filter residue is washed with hexane, yielding the title compound having a melting point of 80°-81° (compound no. 2-1).

1. temperatureWith cooling at 10°
2. concentrationconcentrated by evaporation in vacuo
3. washthe toluene phase is washed with water
4. dry with materialdried over sodium sulfate and 90-95% of the amount of toluene
5. customis evaporated off in vacuo
6. temperatureWhile the mixture is still warm
7. additiona small amount of hexane is added
8. customto crystallise out
9. temperatureThe mixture is cooled
10. filtrationfiltered
11. washthe filter residue is washed with hexane