Ammonium Hydroxide → HCID 13386059, compound

HRID 2290744Notes

Reaction equation

HRID 2290744 reaction equation
Cl[S:2]([C:5]1[CH:10]=[CH:9][C:8]([C:11]2[CH:12]([CH3:18])[NH:13][C:14](=[O:17])[NH:15][N:16]=2)=[CH:7][CH:6]=1)(=[O:4])=[O:3].[OH-].[NH4+:20]>>[S:2]([C:5]1[CH:10]=[CH:9][C:8]([C:11]2[CH:12]([CH3:18])[NH:13][C:14](=[O:17])[NH:15][N:16]=2)=[CH:7][CH:6]=1)(=[O:4])(=[O:3])[NH2:20]

Participants

3

Reactant 2

HCID 14923Ammonium HydroxideHCID 20230169HCID 20230169, compound

Product 1

HCID 13386059HCID 13386059, compound

Procedure

A mixture of 6-(4-chlorosulfonylphenyl)-5-methyl-4,5-dihydro-1,2,4-triazin-3(2H)-one (4.27 g) and concentrated ammonium hydroxide (30 ml) was stirred at room temperature for 30 minutes and then at 50° C. for 1 hour, and concentrated under reduced pressure. To the residue was added water and the mixture was stirred with ice-cooling for 10 minutes. The crystals which formed were recovered by filtration, washed with water and recrystallized from aqueous ethanol to give 6-(4-sulfamoylphenyl)-5-methyl-4,5-dihydro-1,2,4-triazin-3(2H)-one (2.91 g).

Workup

  1. waitat 50° C. for 1 hour
  2. concentrationconcentrated under reduced pressure
  3. additionTo the residue was added water
  4. stirringthe mixture was stirred with ice-
  5. temperaturecooling for 10 minutes
  6. customThe crystals which formed
  7. filtrationwere recovered by filtration
  8. washwashed with water
  9. customrecrystallized from aqueous ethanol

Sources & evidence

ORD record
ord-56cb5992670840c9bb94c666ee297c6c
Source dataset
uspto-grants-1986_10
Patent number
US04618610

Reaction notes

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