HRID963127

反应详情

EQUATION

反应方程式

HRID 963127 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a solution of N-(2-hydroxyethyl)maleimide (0.2 g, 1.41 mmol) in dry dichloromethane (10 ml) and triethylamine (0.22 ml, 1.57 mmol) at 0° C. was added chlorotrimethylsilane (TMS-C1, 0.2 ml, 1.57 mmol). After stirring for 1 hour at room temperature, TLC analysis (ethyl acetate/petroleum ether 1:1) indicated one spot (Rf=0.67). Solvent was removed in vacuo and the residue was dissolved in dichloromethane and filtered through a small silica gel column eluting with dichloromethane. The fractions containing product were pooled and evaporated in vacuo to afford N-(2-trimethylsiloxyethyl)-maleimide (formula H) as colorless flakes (0.3 g; 100% yield).

WORKUP

后处理

  1. customSolvent was removed in vacuo
  2. dissolutionthe residue was dissolved in dichloromethane
  3. filtrationfiltered through a small silica gel column
  4. washeluting with dichloromethane
  5. additionThe fractions containing product
  6. customevaporated in vacuo