Acetic Acid → HCID 15435162, compound

HRID 399418Notes

Reaction equation

HRID 399418 reaction equation
[C:1]([C:4]1[CH2:8][C:7](=[O:9])[N:6]([C:10]2[CH:15]=[CH:14][C:13]([S:16]([NH2:19])(=[O:18])=[O:17])=[CH:12][CH:11]=2)[N:5]=1)(=[O:3])[CH3:2].C(O)(=[O:22])C>>[CH3:8][C:4]1[C:1](=[O:3])[C:2](=[O:22])[C:7](=[O:9])[N:6]([C:10]2[CH:11]=[CH:12][C:13]([S:16]([NH2:19])(=[O:17])=[O:18])=[CH:14][CH:15]=2)[N:5]=1

Participants

3

Procedure

To a suspension of 1.5 g. (4.09 mmole) of 4-(3-acetyl-5-oxo-2-pyrazolin-1-yl)benzene sulfonamide in 5 ml. of acetic acid was added 1.94 g. (12 mmoles) of FeCl3 and the mixture was heated to 90° for 12 hours. After cooling, the solids were collected by filtration and washed with water and dried. The material was then dissolved in 10 ml. of water and triethylamine and 2 g. of sodium sulfide added. After 2 hours, the mixture was acidified with 6 N hydrochloric acid and the solid collected by centrifugation, there was obtained 1.1 g. of material.

Workup

  1. additionTo a suspension of 1.5 g
  2. temperatureAfter cooling
  3. filtrationthe solids were collected by filtration
  4. washwashed with water
  5. customdried
  6. dissolutionThe material was then dissolved in 10 ml
  7. additionof sodium sulfide added
  8. customthe solid collected by centrifugation
  9. customthere was obtained 1.1 g

Sources & evidence

ORD record
ord-4b6c068e2b1b4c83bc72baa1f5ff8ed1
Source dataset
uspto-grants-1998_10
Patent number
US05821243

Reaction notes

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