HRID539986

反应详情

EQUATION

反应方程式

HRID 539986 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

PROCEDURE

实验过程

To a solution of trans-3-tert-butoxycarbonylamino-4-hydroxy-pyrrolidine-1-carboxylic acid benzyl ester (3.9 g) in methanol (31 mL) and tetrahydrofuran (7 mL) was added palladium hydroxide (20 wt % Pd on carbon, 500 mg) and the mixture was stirred at room temperature under 40-45 psi of hydrogen atmosphere overnight. The resulting mixture was filtered and the filtrate was concentrated in vacuo. The residue was triturated in the mixture of ethyl acetate and diisopropylether and filtered to remove the insoluable materials. The filtrate was concentrated in vacuo to afford 2.0 g of trans-tert-butyl [4-hydroxypyrrolidin-3-yl]carbamate (yield was 94%) as a powder. MS obsd. (ESI+) [(M+H)+] 203.

WORKUP

后处理

  1. filtrationThe resulting mixture was filtered
  2. concentrationthe filtrate was concentrated in vacuo
  3. customThe residue was triturated in the mixture of ethyl acetate and diisopropylether
  4. filtrationfiltered
  5. customto remove the insoluable materials
  6. concentrationThe filtrate was concentrated in vacuo