HRID1447560
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- temperatureunder reflux for 2 hr
- filtration, filtered while hot,
- temperaturecooled
- additiondiluted with water
- filtrationThe crude product was filtered off
- customrecrystallised three times from methanol
- customdried at 80° C. in vacuo