HRID1786168

反应详情

EQUATION

反应方程式

HRID 1786168 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a well stirred slurry of 9-chloro-2-cyclopropyl-6H-[1,2,4]triazolo[1,5-c]quinazolin-5-one (5.20 g, 19.9 mmol) in ethylene glycol (40 mL) which was heated to 100° C. was added aqueous sodium hydroxide (10 N, 4 mL, 39.9 mmol). The slurry was heated at reflux for 18 h. After cooling, water (25 mL) was added to the resulted suspension and the pH was adjusted to 6-7 by adding glacial acetic acid (CO2-evolution). The slurry was stirred for 30 min. The solid was collected by filtration and washed with water (3×15 mL). Drying (HV) afforded the title compound (4.05 g, 86%) as a light brown solid. MS: m/e=235.0 [M+H]+.

WORKUP

后处理

  1. temperatureThe slurry was heated
  2. temperatureat reflux for 18 h
  3. temperatureAfter cooling
  4. filtrationThe solid was collected by filtration
  5. washwashed with water (3×15 mL)
  6. customDrying (HV)