反应详情

tert-Butyl methyl(1-((2-(pyrrolidin-1-yl)pyridin-4-yl)methyl)piperidin-4-yl)carbamate (1.469 mmol, 1.0 eq) was dissolved in ethanol (5 ml), and acetyl chloride (7.345 mmol, 5 eq) was added, while cooling with ice. The reaction mixture was stirred for 16 h at RT. TLC monitoring showed that the reaction was incomplete. Acetyl chloride (1 eq) was metered in, and the reaction mixture was stirred for 1 h at 50° C. A solid precipitated. Ethanol was concentrated slightly, and the precipitate was filtered off, washed with diethyl ether and dried. Yield: >99%

1. temperaturewhile cooling with ice
2. stirringwas stirred for 1 h at 50° C
3. customA solid precipitated
4. concentrationEthanol was concentrated slightly
5. filtrationthe precipitate was filtered off
6. washwashed with diethyl ether
7. customdried