HRID4986

反应详情

EQUATION

反应方程式

HRID 4986 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

  1. temperatureThis mixture is heated
  2. temperatureto reflux for 6 hours
  3. customReaction progress
  4. customIf reaction
  5. temperatureat reflux for 2 hours
  6. customMethanol is then removed under reduced pressure
  7. customProduct is recovered
  8. temperatureafter raising the pH of the suspension to 7
  9. additionby addition of NaOH at 0.4°
  10. filtrationfollowed by filtration