HRID1045782

反应详情

EQUATION

反应方程式

HRID 1045782 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

Add palladium/carbon (5%, 1.76 g, 0.8 mmol) in one portion to a solution of benzyl (2S)-2-(4,4,4-trifluorobutanoylamino)propanoate (8.80 g, 29 mmol) in methanol (88 mL) at ambient temperature. Degas the mixture (vacuum/nitrogen), fill with hydrogen (one atmosphere) and stir under hydrogen (29 mmol) for 5 hours. Filter through Celite®, rinse filter cake with methanol and concentrate the filtrate to obtain the title compound as a white solid (6.11 g, 28.7 mmol, 99%). MS (m/z): 214 (M+1); [α]Na25=−24.7° (c=5.0, methanol).

WORKUP

后处理

  1. customDegas the mixture (vacuum/nitrogen)
  2. filtrationFilter through Celite®
  3. washrinse
  4. filtrationfilter cake with methanol
  5. concentrationconcentrate the filtrate