HRID2108799

反应详情

EQUATION

反应方程式

HRID 2108799 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

(3S,4R)-1-Benzyl-3-cyclopropylaminomethyl-4-methylpyrrolidine (25.0 g) was dissolved in ethanol (200 mL). To this solution, trifluoroacetic acid (15.7 mL) and 10% palladium carbon (12.5 g) were added and the mixture was stirred at room temperature under hydrogen pressure of 3.9×105 Pa for 9 hours. The catalyst in the reaction mixture was filtered and the collected catalyst was washed with a 25% aqueous ethanol (300 mL). The filtrate and the washings were combined and concentrated under reduced pressure. The remaining pale brown crystals were suspended in tetrahydrofuran (100 mL) and were filtered. The collected crystals were washed with tetrahydrofuran and dried under reduced pressure to give (3R,4R)-3-cyclopropylaminomethyl-4-methylpyrrolidine-trifluoroacetate as white crystals (34.1 g).

WORKUP

后处理

  1. filtrationThe catalyst in the reaction mixture was filtered
  2. washthe collected catalyst was washed with a 25% aqueous ethanol (300 mL)
  3. concentrationconcentrated under reduced pressure
  4. filtrationwere filtered
  5. washThe collected crystals were washed with tetrahydrofuran
  6. customdried under reduced pressure