HRID465685

反应详情

EQUATION

反应方程式

HRID 465685 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

2-Mercaptoacetamide (10.0 g) and methyl 2-chloroacrylate (13.24 g) were dissolved in warm acetone (100 ml), and potassium carbonate (7.58 g) was added in one portion. Heat was evolved. The mixture was heated to reflux for 2 hours. The red solution was filtered hot using a filter aid, and the residue washed with hot acetone (×2). The filtrate and washings were combined and evaporated to obtain the title compound as a red oil (19.92 g) 1H n.m.r. δ (CDCl3 /DMSO-d6) 3.05-3.18 (4H, overlapping s and d, CH2COR and CH2CH) 3.76 (3H,s,CO2Me), 4.67 (1H,t, J=7Hz, CHCH2), 6.92 (1H, br s, CONH), 7.43 (1H, br s, CONH).

WORKUP

后处理

  1. temperatureHeat
  2. temperatureThe mixture was heated
  3. temperatureto reflux for 2 hours
  4. filtrationThe red solution was filtered hot
  5. washthe residue washed with hot acetone (×2)
  6. customevaporated