Acetic Acid → HCID 15435162, compound

HRID 1584745Notes

Reaction equation

HRID 1584745 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

Reactant 2

HCID 176Acetic AcidHCID 70248236HCID 70248236, compound

Product 1

HCID 15435162HCID 15435162, compound

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° C. 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 6N 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-3c4978b60a3345c08f6b7b2e16bcb9f6
Source dataset
uspto-grants-1999_08
Patent number
US05935957

Reaction notes

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