反应详情

A mixture comprising 5.8 g of 63% sodium hydride, 25 ml of tetrahydrofuran and 10 ml of liquid paraffin, was heated, and a mixture comprising 13.5 g of 4-tert-butylbenzyl cyanide and 15.0 g of 2-trifluoromethylbenzoyl chloride, was dropwise added thereto over a period of 2 hours at a temperature of from 65 to 70° C. After completion of the dropwise addition, the reaction was carried out for 2 hours at the same temperature. The reaction mixture was left to cool to room temperature, and 250 ml of water was poured into the solution. Then, 80 ml of n-hexane was poured, followed by stirring and washing for 10 minutes, and the mixture was left to stand still for 30 minutes, whereupon the aqueous layer was separated and obtained. To the aqueous layer, 8.3 g of concentrated hydrochloric acid was gradually dropwise added with stirring, followed by further stirring for 30 minutes. Precipitated crystals were collected by filtration and washed with 100 ml of water, and then dried at 55° C. for 24 hours to obtain 23.8 g of the desired product. The NMR spectrum data of this product were the same as in Reference Preparation Example 1.

1. temperaturewas heated
2. additionAfter completion of the dropwise addition
3. waitthe reaction was carried out for 2 hours at the same temperature
4. waitThe reaction mixture was left
5. washwashing for 10 minutes
6. waitthe mixture was left
7. waitto stand still for 30 minutes, whereupon the aqueous layer
8. customwas separated
9. customobtained
10. stirringwith stirring
11. stirringby further stirring for 30 minutes
12. customPrecipitated crystals
13. filtrationwere collected by filtration
14. washwashed with 100 ml of water
15. customdried at 55° C. for 24 hours