反应详情

温度

0 °C

1,1-Dimethylethyl 4-[(2-amino-4-chloro-5-methoxyphenyl)amino]-1-piperidinecarboxylate (D48) (280 mg) was dissolved in 5 ml of dichloromethane at 0° C. and phosgene (20% in toluene, 0.5 ml) and triethylamine (0.3 ml) were added and the mixture was stirred at 0° C. for 1 h, then washed with aqueous citric acid, then water, dried over MgSO4, filtered and evaporated The product was chromatographed on silica gel eluting with methanol-dichloromethane mixtures, crystallised from diethyl ether, and then further purified by MDAP to yield the title compound, 40 mg.

1. washwashed with aqueous citric acid
2. dry with materialwater, dried over MgSO4
3. filtrationfiltered
4. customevaporated The product
5. customwas chromatographed on silica gel eluting with methanol-dichloromethane mixtures
6. customcrystallised from diethyl ether
7. customfurther purified by MDAP