反应详情

Methanol (50 ml) was added to an Erlenmeyer flask and acetic acid was added under stirring until pH 5. Methylbenzylamine (1.0 g, 8.8 mmol) and 1-Methyl-4-piperidone (1.1 g, 8.8 mmol) were added to a 100 ml round-bottomed flask and dissolved in the methanol/acetic acid (40 ml) solution previously made. The reaction mixture was stirred for 5 min and NaCNBH3 (0.83 g, 13.2 mmol) was added slowly under stirring. After 20 hours the reaction was concentrated and transferred to a separatory funnel containing dichloromethane and distilled water. The aqueous phase was made basic by addition of Na2CO3. The aqueous phase was extracted twice with dichloromethane. The combined organic layers were collected and dried with Na2SO4. Concentration afforded the title compound. Yield (crude): 98%. UV/MS 89/88 (M+ 353), tr (A, MS) 3.982.

1. additionwas added
2. stirringThe reaction mixture was stirred for 5 min
3. stirringunder stirring
4. concentrationAfter 20 hours the reaction was concentrated
5. customtransferred to a separatory funnel
6. additioncontaining dichloromethane
7. distillationdistilled water
8. additionThe aqueous phase was made basic by addition of Na2CO3
9. extractionThe aqueous phase was extracted twice with dichloromethane
10. customThe combined organic layers were collected
11. dry with materialdried with Na2SO4
12. concentrationConcentration