HRID4118

反应详情

EQUATION

反应方程式

HRID 4118 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
0 °C

PROCEDURE

实验过程

N-(2-Oxo-1-imidazolidinyl)carbamic acid, 1,1-dimethylethyl ester (12.0 g, 0.06 mmol) was dissolved in dichloromethane (75 ml) containing pyridine (5.2 g, 0.066 mol). The solution was cooled to 0° C. and treated slowly with bromoacetyl bromide (13.3 g, 0.066 mol). The solution was evaporated in vacuo to give a yellow oil. The oil was chromatographed on silica gel (~300 g) eluting with 10% ethyl acetate/dichloromethane. The appropriate fractions were combined and evaporated in vacuo to give the title compound as a white solid, 16.7 g.

WORKUP

后处理

  1. customThe solution was evaporated in vacuo
  2. customto give a yellow oil
  3. customThe oil was chromatographed on silica gel (~300 g)
  4. washeluting with 10% ethyl acetate/dichloromethane
  5. customevaporated in vacuo