反应详情

温度

70 °C

To a solution of 1.03 mmol 3-hydroxy-pyrrolidine-1-carboxylic acid tert-butyl ester in 15 ml tetrahydrofuran were added successively 1.23 mmol 4-hydroxybenzotrifluoride, 1.43 mmol triphenylphosphine and 1.43 mmol di-tert-butyl azodicarboxylate. The reaction mixture was stirred at 70° C. for 28 h and was then cooled to room temperature and concentrated in vacuo. The crude material was purified by chromatography (ethyl acetate/heptane) to afford the title compound as a white crystalline solid (yield 15%). MS (m/e): 276.1 ([M+H-Me2C═CH2]+, 100%).

1. temperaturewas then cooled to room temperature
2. concentrationconcentrated in vacuo
3. customThe crude material was purified by chromatography (ethyl acetate/heptane)