HRID358900

反应详情

EQUATION

反应方程式

HRID 358900 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

6.3 ml of 6N aqueous hydrochloric acid were added to a solution of 0.4 g (0.0019 mole) of 3-amino-1-t-butoxycarbonyl-4-methoxypyrrolidine [prepared as described in Step (3) above] dissolved in 20 ml of ethanol, and the mixture was heated under reflux for 1.5 hours, after which the solvent was removed by evaporation under reduced pressure. The residue was washed with a 1:9 by volume mixture of ethanol and ethyl acetate to give 0.34 g of trans-3-amino-4-methoxypyrrolidine dihydrochloride as a colorless powder, melting at 248°~258° C. (with decomposition).

WORKUP

后处理

  1. temperaturethe mixture was heated
  2. temperatureunder reflux for 1.5 hours
  3. customafter which the solvent was removed by evaporation under reduced pressure
  4. washThe residue was washed with a 1:9 by volume mixture of ethanol and ethyl acetate