Sodium Carbonate → HCID 430947, compound

HRID 1604986Notes

Reaction equation

HRID 1604986 reaction equation
Cl.NO.C(=O)([O-])[O-:5].[Na+].[Na+].Cl.[O:11]1[C:15]2[CH:16]=[CH:17][CH:18]=[CH:19][C:14]=2[C:13]([CH2:20][C:21]([NH2:23])=[NH:22])=[N:12]1>O.C(O)C>[O:11]1[C:15]2[CH:16]=[CH:17][CH:18]=[CH:19][C:14]=2[C:13]([CH2:20][C:21](=[N:23][OH:5])[NH2:22])=[N:12]1

Participants

6

Reactant 3

HCID 10340Sodium CarbonateHCID 443297Hydroxyamine hydrochlorideHCID 12279048HCID 12279048, compound

Product 1

HCID 430947HCID 430947, compoundYield 84.3%

Reagents, catalysts & solvents 2

HCID 702EthanolSolventHCID 962WaterSolvent

Conditions

Temperature
80 °C

Procedure

To a solution of hydroxylamine hydrochloride (0.17 g) and sodium carbonate (0.13 g) in water (5 ml) was added a solution of 1,2-benzisoxazole-3-acetamidine hydrochloride (0.21 g) in ethanol (10 ml) and the mixture was heated on water bath at 80°C for 1 hour. The solvent was distilled off under a reduced pressure and to the residue was added water. The mixture was made alkaline with sodium bicarbonate and the precipitated crystalline were separated by filtration, washed with water, dried and recrystallized from ethanol to give the desired compound (0.16 g). m.p. 160° to 162°C.

Workup

  1. distillationThe solvent was distilled off under a reduced pressure and to the residue
  2. additionwas added water
  3. customthe precipitated crystalline were separated by filtration
  4. washwashed with water
  5. customdried
  6. customrecrystallized from ethanol

Sources & evidence

ORD record
ord-cae5eae2132949d8bf90c1bdd5030985
Source dataset
uspto-grants-1976_04
Patent number
US03948928

Reaction notes

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