HRID451451

反应详情

EQUATION

反应方程式

HRID 451451 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-(3-bromo-6-ethoxycarbonyl-pyridin-2-yl)-N′-ethoxycarbonyl-thiourea (2 g, 5.52 mmol) in dry methanol (10 mL) were added hydroxylamine hydrochloride (1.92 g, 27.62 mmol) and diisopropyl ethylamine (2.98 mL, 16.57 mmol) under an argon atmosphere and stirred at room temperature for 4 hours. The solid was filtered and methanol (40 mL) was added to residue. The reaction mixture was heated to reflux for 12 hours. The solvent was evaporated and the title compound was obtained as off white solid (800 mg, 53%).

WORKUP

后处理

  1. filtrationThe solid was filtered
  2. additionmethanol (40 mL) was added to residue
  3. temperatureThe reaction mixture was heated
  4. temperatureto reflux for 12 hours
  5. customThe solvent was evaporated