HRID606448

反应详情

EQUATION

反应方程式

HRID 606448 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
100 °C

PROCEDURE

实验过程

A mixture of ethyl 1H-1,2,4-triazol-3-ylacetate obtained in Reference Example 14 (900 mg, 5.80 mmol), 4N aqueous sodium hydroxide solution (7.25 mL, 29.0 mmol), water (10 mL), methanol (10 mL) and THF (10 mL) was stirred at 100° C. for 2 hr. The reaction mixture was concentrated under reduced pressure, the residue was acidified with 1N hydrochloric acid, and the mixture was concentrated under reduced pressure. Ethanol was added to the residue, and the insoluble material was filtered off, and the filtrate was concentrated. The residue was crystallized from toluene to give the title compound as a white powder (369 mg, 50%).

WORKUP

后处理

  1. concentrationThe reaction mixture was concentrated under reduced pressure
  2. concentrationthe mixture was concentrated under reduced pressure
  3. additionEthanol was added to the residue
  4. filtrationthe insoluble material was filtered off
  5. concentrationthe filtrate was concentrated
  6. customThe residue was crystallized from toluene