反应详情

温度

50 °C

29 g (146.5 mmol) diphosgene in 300 ml 1,2-dichlorethane were treated at −20° C. with a solution of 13 g (58.6 mmol) 3-nitro-4-(trifluormethoxy)-aniline in 20 ml 1,2-dichlorethane. The mixture was allowed to come to room temperature and then was heated to 50° C. for 3 h. After standing over night, the solvent was evaporated and the residual oil was taken up in 250 ml THF. 13 g (58.6 mmol) 2-methyl-2-[(pyridin-4-ylmethyl)-amino]-propionic acid methyl ester in 250 ml THF were added and the mixture was heated to 40° C. for 1 h. The solvent was evaporated and the residue purified by flash chromatography (Silica gel, methylene chloride:methanol=95:5). Yield: 19.7 g.

1. customto come to room temperature
2. waitAfter standing over night
3. customthe solvent was evaporated
4. temperaturethe mixture was heated to 40° C. for 1 h
5. customThe solvent was evaporated
6. customthe residue purified by flash chromatography (Silica gel, methylene chloride:methanol=95:5)