HRID1295374

反应详情

EQUATION

反应方程式

HRID 1295374 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

To Intermediate 41, the more polar isomer (1S,2S)-3-benzyl-2-phenyl-3-aza-bicyclo[3.1.0]hexane-1-carboxylic acid [(S)-1-(3,5-bis-trifluoromethyl-phenyl)-ethyl]-methyl-amide (0.06 g, 0.11 mmol) was combined with palladium on carbon 20% (Pearlman's catalyst, 0.08 g) and HOAc (8 mL) and hydrogenated at 40 psi for 16 hours. The material was filtered thru celite and concentrated, then partitioned between saturated sodium bicarbonate solution and methylene chloride, the organics were washed with brine, dried over sodium sulfate, filtered, and concentrated. The crude material was purified via prep tic using ETOAc as the eluant to give the title compound (0.027 g, 54% yield).

WORKUP

后处理

  1. filtrationThe material was filtered thru celite
  2. concentrationconcentrated
  3. custompartitioned between saturated sodium bicarbonate solution and methylene chloride
  4. washthe organics were washed with brine
  5. dry with materialdried over sodium sulfate
  6. filtrationfiltered
  7. concentrationconcentrated
  8. customThe crude material was purified via prep tic