反应详情

The solution of 15.1 g of 3-acetonyl-4-(3,4-dimethoxyphenyl)-1,5,6,7-tetrahydro-2H-azepinone, 25.5 ml of isopropylamine 10 ml of 5.8 N methanolic hydrogen chloride and 3.4 g of sodium cyanoborohydride in 260 ml of methanol is refluxed for 3 days. The mixture is cooled, acidified to pH=1 with concentrated hydrochloric acid, evaporated and the residue diluted with water. It is washed with ether, basified with 3 N aqueous sodium hydroxide to pH=11 and extracted with diethyl ether. The extract is dried, evaporated and the residue dissolved in 75 ml of acetone. The solution is treated with 4.4 N ethanolic hydrogen chloride, and the precipitate collected, to yield the 3-(2-isopropylaminopropyl)-4-(3,4-dimethoxyphenyl)-1,5,6,7-tetrahydro-2H-azepinone hydrochloride monohydrate melting at 135°-138°.

1. temperatureThe mixture is cooled
2. customevaporated
3. additionthe residue diluted with water
4. washIt is washed with ether
5. extractionextracted with diethyl ether
6. customThe extract is dried
7. customevaporated
8. dissolutionthe residue dissolved in 75 ml of acetone
9. additionThe solution is treated with 4.4 N ethanolic hydrogen chloride
10. customthe precipitate collected