HRID630272

反应详情

EQUATION

反应方程式

HRID 630272 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a refluxing solution of thiourea (2.6 g, 34.3 mmol) in absolute ethanol (30 mL) was added ethyl 2-bromo-3-oxopentanoate (7.3 g, 32.7 mmol) always keeping the mixture at reflux. The solution was stirred at reflux for another 1.5 hours. After cooling to room temperature, the solution was poured in ice/water (150 mL). The mixture was neutralized with concentrated NH4OH. The solid material was recovered by filtration, washed with water (2×50 mL) and hexanes (3×50 mL), and dried in vacuo, affording ethyl 2-amino-4-ethyl-1,3-thiazole-5-carboxylate (6.8 g, 94% yield). The product was used without further purification.

WORKUP

后处理

  1. temperatureat reflux
  2. temperatureat reflux for another 1.5 hours
  3. filtrationThe solid material was recovered by filtration
  4. washwashed with water (2×50 mL) and hexanes (3×50 mL)
  5. customdried in vacuo