HRID1451958

反应详情

EQUATION

反应方程式

HRID 1451958 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

The CBZ group of (S)-phenylmethyl-[1-methyl-2-oxo-2(1H-pyrrol-1-ylamino)ethyl]carbamate (5.50 g) was cleaved in a minimal volume of methanol over 5% Pd-C (0.83 g) with H2 (g) (468 ml) under atmospheric conditions. The catalyst was removed by filtration through a pad of celite and the filter cake was washed with methanol. The combined filtrate was concentrated and the residue purified via flash column chromatography (silica gel, 20% EtOH/ethyl acetate) to afford 2.62 g of the desired product as an oil which crystallized on standing, m.p. 81°-82° C.

WORKUP

后处理

  1. customThe catalyst was removed by filtration through a pad of celite
  2. washthe filter cake was washed with methanol
  3. concentrationThe combined filtrate was concentrated
  4. customthe residue purified via flash column chromatography (silica gel, 20% EtOH/ethyl acetate)