反应详情

1-(1 phenylcyclohexyl)-4 piperidone (0.245 q) and ammonium acetate (I q) were dissolved in 3.5 mL dry methanol. After stirring at room temperature for 10 minutes, sodium cyanoborohydride (0.1 q) was added and the reaction was stoppered. After 20 hours, 0.1 mL of concentrated hydrochloric acid was added followed by 10 mL water and the mixture was stirred for 1.5 hours. The solution was basified with potassium carbonate to pH 9 and extracted with methylene chloride. The methylene chloride was dried over Na2SO4 and removed in vacuo. The product distilled as a colorless, clear oil at 90°-130° C. in vacuo (about 5 mmHg).

1. waitAfter 20 hours
2. stirringthe mixture was stirred for 1.5 hours
3. extractionextracted with methylene chloride
4. dry with materialThe methylene chloride was dried over Na2SO4
5. customremoved in vacuo
6. distillationThe product distilled as a colorless, clear oil at 90°-130° C. in vacuo (about 5 mmHg)