HRID56430

反应详情

EQUATION

反应方程式

HRID 56430 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A mixture of Racemate-ethyl 3-(benzyloxycarbonylamino)-4-((2-(trimethylsilyl)ethoxy)carbonylamino)cyclohexanecarboxylate (1.7 g, 3.7 mmol) and 5% palladium on carbon (50% wet, 300 mg) in isopropanol (35 mL) was stirred under 1 atm hydrogen atmosphere at room temperature for 18 hours. The mixture was filtered through a pad of celite. The filtrate was concentrated and purified by silica gel chromatography (methanol/dichloromethane=1/30 to 1/10) to afford the title compound (1.0 g, 89%) as a yellow oil. MS (ES+) C15H30H2O4Si requires: 330, found: 331 [M+H]+.

WORKUP

后处理

  1. filtrationThe mixture was filtered through a pad of celite
  2. concentrationThe filtrate was concentrated
  3. custompurified by silica gel chromatography (methanol/dichloromethane=1/30 to 1/10)