HRID452593

反应详情

EQUATION

反应方程式

HRID 452593 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A suspension of 1H-indazole-5-carbohydrazide (4.40 g, 25.0 mmol), carbon disulfide (3.76 mL, 62.5 mmol) and triethylamine (4.18 mL, 30.0 mmol) in ethanol (100 mL) was heated under reflux for 7 hr. After cooling, the reaction mixture was poured into water, and acidified with 1M hydrochloric acid. The precipitate was collected by filtration, dried and recrystallized from tetrahydrofuran to give the title compound (5.27 g, yield 97%) as colorless crystals.

WORKUP

后处理

  1. temperaturewas heated
  2. temperatureunder reflux for 7 hr
  3. temperatureAfter cooling
  4. filtrationThe precipitate was collected by filtration
  5. customdried
  6. customrecrystallized from tetrahydrofuran