Methanol → HCID 21430498, compound

HRID 437157Notes

Reaction equation

HRID 437157 reaction equation
Cl.[CH3:2][N:3]([CH3:23])[S:4]([C:7]1[CH:8]=[C:9]([CH:13]=[CH:14][C:15]=1[N:16]1[CH2:21][CH2:20][N:19]([CH3:22])[CH2:18][CH2:17]1)[C:10](Cl)=[O:11])(=[O:6])=[O:5].[CH3:24][OH:25]>>[CH3:24][O:25][C:10](=[O:11])[C:9]1[CH:13]=[CH:14][C:15]([N:16]2[CH2:21][CH2:20][N:19]([CH3:22])[CH2:18][CH2:17]2)=[C:7]([S:4](=[O:5])(=[O:6])[N:3]([CH3:23])[CH3:2])[CH:8]=1

Participants

3

Reactant 2

HCID 887MethanolHCID 21430472HCID 21430472, compound

Product 1

HCID 21430498HCID 21430498, compound

Procedure

40 Grams of 3-dimethylsulfamoyl-4-(4-methylpiperazine-1-yl)-benzoylchloride-hydrochloride (0.1 mole) were heated for 2 hours under reflux in 1 l of methanol. Subsequently the methanol was distilled off and the residue was dissolved in 0.3 l of water. A small amount of undissolved amorphous material was removed by filtration and the pH value of the filtrate was adjusted to 8 by means of concentrated aqueous ammonia, whereupon the final product precipitated immediately in a crystalline state. After it had been washed with water, it was dried on the steam bath.

Workup

  1. distillationSubsequently the methanol was distilled off
  2. dissolutionthe residue was dissolved in 0.3 l of water
  3. customA small amount of undissolved amorphous material was removed by filtration
  4. customprecipitated immediately in a crystalline state
  5. washAfter it had been washed with water, it
  6. customwas dried on the steam bath

Sources & evidence

ORD record
ord-fa08cefda6f74cd4b135741d7c4ecf06
Source dataset
uspto-grants-1977_06
Patent number
US04029787

Reaction notes

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