反应详情

温度

80 °C

A flask was charged with [1-(3-methoxy-phenyl)-1-methyl-ethyl]-carbamic acid benzyl ester (D100) (1 g, 3.34 mmol, 1 equiv), 10% palladium on charcoal (50% wet, 100 mg, 10% w/w), NH4COOH (2.1 g, 33 mmol, 10 equiv), EtOH (40 ml) and H2O (8 ml). The resulting mixture was stirred at 80° C. for 2 h, cooled to room temperature and the catalyst was filtered off using a pad of celite. Most of the EtOH was removed in vacuo and the residue was diluted with 1N HCl aqueous solution. The aqueous phase was extracted with AcOEt then basified to pH 13 and extracted twice with AcOEt. These combined organic layers were dried over MgSO4 and concentrated in vacuo to yield 1-(3-methoxy-phenyl)-1-methyl-ethylamine (F15) (290 mg, 53%) as a yellow gum.

1. temperaturecooled to room temperature
2. filtrationthe catalyst was filtered off
3. customMost of the EtOH was removed in vacuo
4. additionthe residue was diluted with 1N HCl aqueous solution
5. extractionThe aqueous phase was extracted with AcOEt
6. extractionextracted twice with AcOEt
7. dry with materialThese combined organic layers were dried over MgSO4
8. concentrationconcentrated in vacuo