反应详情

温度

10 °C

To a stirred two phase solution of 1,2-diphenylethylamine (30.0 g, 0.15 mol) in 300 ml of methylene chloride and 500 ml of water was added sodium carbonate (23.9 g, 0.225 mol) and the solution was cooled to 10° C. under nitrogen. Ethyl chloroformate (21.5 ml, 0.225 mol) was added dropwise over a 1 hour period. The reaction was warmed to ambient temperature and stirred at that temperature for 3 hours. The phases were separated and the aqueous phase was extracted with methylene chloride (75 ml). The combined methylene chloride extracts were washed with 1N HCl (200 ml), dried and evaporated to a white solid, 40.3 g. Recrystallization from cyclohexane gave N-carboethoxy-1,2-diphenylethylamine, mp 74°-75° C.

1. temperatureThe reaction was warmed to ambient temperature
2. customThe phases were separated
3. extractionthe aqueous phase was extracted with methylene chloride (75 ml)
4. washThe combined methylene chloride extracts were washed with 1N HCl (200 ml)
5. customdried
6. customevaporated to a white solid, 40.3 g
7. customRecrystallization from cyclohexane