HRID504158

反应详情

EQUATION

反应方程式

HRID 504158 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Lithium aluminum hydride (0.95 mL of a 1.0 M solution in THF, 0.95 mmoles) was added to a room temperature solution of [(S)-1-(Methoxy-methyl-carbamoyl)-2-phenyl-ethyl]-carbamic acid benzyl ester (0.30 g, 0.86 mmoles) in THF (10 mL). The resulting mixture was stirred at room temperature for 2 h, then was quenched by dilution with EtOAc (200 mL), and washed with 1% aqueous HCl (200 mL). The organic layer was dried (MgSO4) and concentrated in vacuo. The residue was repeatedly diluted with CH3CN (2×200 mL) and concentrated in vacuo to give 0.24 g (approximately quantitative yield) of ((S)-1-Benzyl-2-oxo-ethyl)-carbamic acid benzyl ester as a colorless oil, which was carried on without further purification: ES+ LC/MS m/e 284 (M+H), RT=4.75 min.

WORKUP

后处理

  1. customwas quenched by dilution with EtOAc (200 mL)
  2. washwashed with 1% aqueous HCl (200 mL)
  3. dry with materialThe organic layer was dried (MgSO4)
  4. concentrationconcentrated in vacuo
  5. additionThe residue was repeatedly diluted with CH3CN (2×200 mL)
  6. concentrationconcentrated in vacuo