反应详情

A mixture comprising 5.8 g of 63% sodium hydride and 137 ml of tetrahydrofuran was heated, and a mixture comprising 13.5 g of 4-tert-butylbenzyl cyanide, 15.0 g of 2-trifluoromethylbenzoyl chloride and 50 ml of tetrahydrofuran, was dropwise added thereto over a period of 2 hours under reflux. After completion of the dropwise addition, the reaction was carried out at the same temperature for 2 hours. Tetrahydrofuran in the reaction mixture was distilled off, and 250 ml of water was poured into the residue. Then, 80 ml of n-hexane was added thereto, and the mixture was stirred and washed for 10 minutes and then left to stand for 30 minutes. Then, the aqueous layer was separated. 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 23.7 g of the desired product. The NMR spectrum data of this product were as follows.

1. temperaturewas heated
2. temperatureover a period of 2 hours under reflux
3. additionAfter completion of the dropwise addition
4. distillationTetrahydrofuran in the reaction mixture was distilled off
5. addition250 ml of water was poured into the residue
6. additionThen, 80 ml of n-hexane was added
7. washwashed for 10 minutes
8. waitleft
9. waitto stand for 30 minutes
10. customThen, the aqueous layer was separated
11. additionTo the aqueous layer, 8.3 g of concentrated hydrochloric acid was gradually dropwise added
12. stirringwith stirring
13. stirringby further stirring for 30 minutes
14. customPrecipitated crystals
15. filtrationwere collected by filtration
16. washwashed with 100 ml of water
17. customdried at 55° C. for 24 hours