反应详情

温度

25 °C

To a solution of 10.71 g of 5,6,7,8-tetra-hydro-4H-thieno[3,2-b]azepine and 19.4 ml of triethylamine in 150 ml of dichloromethane under argon is added in small portions 4-nitrobenzoyl chloride (exothermic). The mixture is stirred for 3 hours at 25° C. and then washed with water, sodium bicarbonate solution, brine and dried (Na2SO4). The solvent is removed, the residue dried under vacuum and recrystallized by dissolving in hot ethyl acetate and diluting with hexane. Chilling overnight and filtering gives 16 g of light brown crystals, m.p. 141°-142° C.

1. washwashed with water, sodium bicarbonate solution, brine
2. dry with materialdried (Na2SO4)
3. customThe solvent is removed
4. customthe residue dried under vacuum
5. customrecrystallized
6. dissolutionby dissolving in hot ethyl acetate
7. additiondiluting with hexane
8. temperatureChilling overnight
9. filtrationfiltering