HRID1447560

反应详情

EQUATION

反应方程式

HRID 1447560 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

To 3-(5tetrazolyl)thioxanthone-10,10-dioxide (1.25 g.), zinc wool (2.50 g.) and mercuric acetate (0.10 g.) 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