HRID639122

反应详情

EQUATION

反应方程式

HRID 639122 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Dissolve 1,1-dimethylethyl(3R,4R)-3-hydroxy-4-[({[(phenylmethyl)oxy]carbonyl}amino)methyl]-1-pyrrolidinecarboxylate (1.0 g, 2.85 mmol) in methylene chloride (20 mL). Add PCC (1.23 g, 5.7 mmol) and Florisil (2.5 g) and stir at ambient temperature for 16 hours. Add 3 more equivalents of PCC (1.84 g, 8.55 mmol) and stir for 48 hours. Dilute solution with ether and filter through a pad of celite. The solvent was removed under reduced pressure yielding a crude oil. The crude mixture was purified on silica gel. (0.598 g, 60%). LCMS: m/z 349.4 (MH+).

WORKUP

后处理

  1. filtrationDilute solution with ether and filter through a pad of celite
  2. customThe solvent was removed under reduced pressure
  3. customyielding a crude oil
  4. customThe crude mixture was purified on silica gel