HRID574338

反应详情

EQUATION

反应方程式

HRID 574338 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

To a solution of 3-bromo-1H-pyrazol-5-amine (0.2 g, 1.235 mmol) and dimethyl 2-acetylsuccinate (0.697 g, 3.70 mmol) in xylene (10 mL) was added p-toluenesulfonic acid monohydrate (2 mg, 10.51 μmol). The reaction mixture was heated at reflux under a Dean-Stark trap for 8 h. The solid was filtered and washed with hexanes to afford the title compound (0.201 g, 54.2%). 1H NMR (400 MHz, MeOD) δ 2.37 (3H, s), 3.65 (2H, s), 3.71 (3H, s), 6.20 (1H, s).

WORKUP

后处理

  1. temperatureThe reaction mixture was heated
  2. temperatureat reflux under a Dean-Stark trap for 8 h
  3. filtrationThe solid was filtered
  4. washwashed with hexanes