HRID4986
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
This is prepared by hydrolysis of the acetamide 2-acetylamino-1,3,4-thiadiazole-5-sulfonamide (acetazolamide). A slurry of 0.2 mol of acetazolamide in 600 mL of methanol is treated with 60 mL 12N HCl. This mixture is heated with stirring to reflux for 6 hours. Reaction progress is monitored using liquid chromatography. If reaction is not completed after 6 hours, another 30 mL of 12N HCl is added, and the mixture held at reflux for 2 hours. Methanol is then removed under reduced pressure. Product is recovered after raising the pH of the suspension to 7 by addition of NaOH at 0.4° , followed by filtration. Yield is between 85 and 98% of theoretical with 99% purity. KI =40 nM.
WORKUP
后处理
- temperatureThis mixture is heated
- temperatureto reflux for 6 hours
- customReaction progress
- customIf reaction
- temperatureat reflux for 2 hours
- customMethanol is then removed under reduced pressure
- customProduct is recovered
- temperatureafter raising the pH of the suspension to 7
- additionby addition of NaOH at 0.4°
- filtrationfollowed by filtration