反应详情

温度

0 °C

1,1-Dimethylethyl 4-[(2-amino-5-chloro-4-trifluoromethylphenyl)amino]-1-piperidinecarboxylate (D62, 2.2 g) was dissolved in 25 ml of dichloromethane at 0° C. and triphosgene (0.6 g) and diisopropylethylamine (1.0 ml) were added and the mixture was stirred at 0° C. for 1 h, then washed with aqueous citric acid, dried over MgSO4, filtered and evaporated The product was chromatographed on silica gel eluting with methanol-dichloromethane mixtures, then crystallised from diethyl ether to yield the subtitle compound, 1.0 g.

1. washwashed with aqueous citric acid
2. dry with materialdried over MgSO4
3. filtrationfiltered
4. customevaporated The product
5. customwas chromatographed on silica gel eluting with methanol-dichloromethane mixtures
6. customcrystallised from diethyl ether