반응 #432236

반응 방정식

HCl

acetamide 2-acetylamino-1,3,4-thiadiazole-5-sulfonamide

acetazolamide

HCl

→

2-amino-1,3,4-thiadiazole-5-sulfonamide

수율 85.0%

용매

methanol

반응 조건

후처리

1. 1
   온도This mixture is heated
2. 2
   온도to reflux for 6 hours
3. 3
   기타Reaction progress
4. 4
   기타If reaction
5. 5
   온도at reflux for 2 hours
6. 6
   기타Methanol is then removed under reduced pressure
7. 7
   기타Product is recovered
8. 8
   온도after raising the pH of the suspension to 7
9. 9
   workup.ADDITIONby addition of NaOH at 0° C.-4° C.
10. 10
    여과followed by filtration

실험 절차

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° C.-4° C., followed by filtration. Yield is between 85% and 98% of theoretical with 99% purity. KI =40 nM.

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