HRID1608268

反应详情

EQUATION

反应方程式

HRID 1608268 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of Ethyl 4-[aminomethyl]benzeneacetate (4.12 g) in anhydrous dichloromethane (60 ml) containing triethylamine (3.0 ml), was added over 20 min to a cold (-15°) stirred solution of acryloyl chloride (1.73 ml) in dry dichloromethane (50 ml) and stirring was continued for 0.75 h. After washing the dichloromethane solution with 8% aqueous sodium bicarbonate soln (2×50 ml) and drying (MgSO4), the organic solvent was removed by rotary evaporation to yield a a solid (approximately 6 g) which was triturated with cyclohexane to give the title compound as a solid (4.1 g) m.p. 93°-95°.

WORKUP

后处理

  1. additionwas added over 20 min to a cold (-15°)
  2. washAfter washing the dichloromethane solution with 8% aqueous sodium bicarbonate soln (2×50 ml)
  3. dry with materialdrying (MgSO4)
  4. customthe organic solvent was removed by rotary evaporation