Ammonia → HCID 430947, compound

HRID 1604987Notes

Reaction equation

HRID 1604987 reaction equation
[O:1]1[C:5]2[CH:6]=[CH:7][CH:8]=[CH:9][C:4]=2[C:3]([CH2:10][C:11](Cl)=[N:12][OH:13])=[N:2]1.[NH3:15]>C(Cl)(Cl)Cl.C(O)C>[O:1]1[C:5]2[CH:6]=[CH:7][CH:8]=[CH:9][C:4]=2[C:3]([CH2:10][C:11](=[N:12][OH:13])[NH2:15])=[N:2]1

Participants

5

Reactant 2

HCID 222Ammonia2×HCID 85444374HCID 85444374, compound

Product 1

HCID 430947HCID 430947, compound

Reagents, catalysts & solvents 2

HCID 702EthanolSolventHCID 6212ChloroformSolvent

Procedure

In a mixture of chloroform (250 ml) and ethanol (250 ml) was dissolved 1,2-benzisoxazole-3-acetohydroximic chloride (0.5 g) and the mixture was saturated with ammonia by passing through thereto ammonia gas under ice-cooling. The mixture was allowed to stand for 0.5 hour and then the solvent was distilled off under a reduced pressure. To the residue was added chloroform and the insoluble substance was filtered off. The filtrate was distilled to remove the solvent and the residue was recrystallized from ethanol to give the desired compound (0.38 g). m.p. 161° to 163°C.

Workup

  1. temperaturecooling
  2. distillationthe solvent was distilled off under a reduced pressure
  3. additionTo the residue was added chloroform
  4. filtrationthe insoluble substance was filtered off
  5. distillationThe filtrate was distilled
  6. customto remove the solvent
  7. customthe residue was recrystallized from ethanol

Sources & evidence

ORD record
ord-2da4132c58754ec68a9b151ba4d85daf
Source dataset
uspto-grants-1976_04
Patent number
US03948928

Reaction notes

Loading…