HRID614497

反应详情

EQUATION

反应方程式

HRID 614497 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

To 3-(5-tetrazolyl)thioxanthone-10,10-dioxide (1.25g.), zinc wool (2.50g.) and mercuric acetate (0.10g.) was added acetic acid (25 ml.) and concentrated hydrochloric acid (25 ml.), and the mixture boiled under reflux for 2 hr. After this time a further amount of hydrochloric acid (1.5 ml.) was added and the mixture boiled for a further 4 hr., filtered while hot, cooled, and diluted with water. The crude product was filtered off, recrystallised three times from methanol, and dried at 80° C in vacuo to give 3-(5-tetrazolyl)thioxanthene-10,10-dioxide m.pt. 233° C with decomposition.

WORKUP

后处理

  1. temperatureunder reflux for 2 hr
  2. filtration, filtered while hot,
  3. temperaturecooled
  4. additiondiluted with water
  5. filtrationThe crude product was filtered off
  6. customrecrystallised three times from methanol
  7. customdried at 80° C in vacuo