1-Methylpiperazine → HCID 53722557, compound

HRID 437153Notes

Reaction equation

HRID 437153 reaction equation
Cl[C:2]1[CH:10]=[CH:9][C:5]([C:6]([NH2:8])=[O:7])=[CH:4][C:3]=1[S:11](=[O:14])(=[O:13])[NH2:12].[CH3:15][N:16]1[CH2:21][CH2:20][NH:19][CH2:18][CH2:17]1>O>[CH3:15][N:16]1[CH2:21][CH2:20][N:19]([C:2]2[CH:10]=[CH:9][C:5]([C:6]([NH2:8])=[O:7])=[CH:4][C:3]=2[S:11](=[O:14])(=[O:13])[NH2:12])[CH2:18][CH2:17]1

Participants

4

Reactant 2

HCID 531671-MethylpiperazineHCID 213020Sulclamide [INN:DCF]

Product 1

HCID 53722557HCID 53722557, compound

Reagents, catalysts & solvents 1

HCID 962WaterSolvent

Procedure

165 Grams of 4-chloro-3-sulfamoylbenzoic acid-amide (0.7 mole) were stirred with 0.3 l of N-methylpiperazine for 1 hour at 130° C. Subsequently the reaction mixture was diluted with 2 l of water, and the crystalline precipitate was suction-filtered. The crude product (150 g with a degradation point of 301° C.) was dissolved in 3 l of 0.5N HCl and, after the solution had been decolorized with activated charcoal, the said product was precipitated in a crystalline state, at pH 8, by means of 2N ammonia.

Workup

  1. filtrationthe crystalline precipitate was suction-filtered
  2. dissolutionThe crude product (150 g with a degradation point of 301° C.) was dissolved in 3 l of 0.5N HCl
  3. customthe said product was precipitated in a crystalline state, at pH 8, by means of 2N ammonia

Sources & evidence

ORD record
ord-cd6bff268d9d450ebdaab67fee7823c5
Source dataset
uspto-grants-1977_06
Patent number
US04029787

Reaction notes

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