反应详情

温度

50 °C

A mixture of 4-(4-{[(S)-2-(4-methanesulfonylphenyl)-1-methylethyl]-propylamino}butyl)-3-oxo-[1,4]diazepane-1-carboxylic acid tert-butyl ester (0.9 g, 1.75 mmole) and 3N hydrochloric acid (4 mL) was warmed to 50° C. The reaction mixture was stirred at room temperature for 30 minutes, and the pH was adjusted to 10 with saturated sodium carbonate. The mixture was extracted with ethyl acetate (30 mL), and the organic phase was dried (magnesium sulfate), and concentrated. The residue was dissolved in diethyl ether (10 mL) and 1M hydrogen chloride in diethyl ether (2 mL) was added. The precipitate was collected, washed with diethyl ether and hexane, and dried in vacuo to give 1-(4-{[(S)-2-(-4-methanesulfonyl-phenyl)-1-methylethyl]propylamino}butyl)-[1,4]diazepan-2-one, dihydrochloride salt (0.49 g), 149, M+H=424.

1. extractionThe mixture was extracted with ethyl acetate (30 mL)
2. dry with materialthe organic phase was dried (magnesium sulfate)
3. concentrationconcentrated
4. dissolutionThe residue was dissolved in diethyl ether (10 mL)
5. addition1M hydrogen chloride in diethyl ether (2 mL) was added
6. customThe precipitate was collected
7. washwashed with diethyl ether and hexane
8. customdried in vacuo