Sodium Carbonate → HCID 53772032, compound

HRID 1604980Notes

Reaction equation

HRID 1604980 reaction equation
[CH3:1][O:2][C:3]1[CH:4]=[CH:5][C:6]2[O:10][N:9]=[C:8]([CH2:11][C:12]#[N:13])[C:7]=2[CH:14]=1.Cl.[NH2:16][OH:17].C(=O)([O-])[O-].[Na+].[Na+]>C(O)C.O>[CH3:1][O:2][C:3]1[CH:4]=[CH:5][C:6]2[O:10][N:9]=[C:8]([CH2:11][C:12](=[N:16][OH:17])[NH2:13])[C:7]=2[CH:14]=1

Participants

6

Reactant 3

HCID 10340Sodium CarbonateHCID 443297Hydroxyamine hydrochlorideHCID 12279033HCID 12279033, compound

Product 1

HCID 53772032HCID 53772032, compoundYield 76.6%

Reagents, catalysts & solvents 2

HCID 702EthanolSolventHCID 962WaterSolvent

Procedure

In ethanol (20 ml) was dissolved 5-methoxy-1,2-benzisoxazole-3-acetonitrile (2.0 g) and thereto was added a solution of hydroxylamine hydrochloride (0.88 g) and sodium carbonate (1.34 g) in water (10 ml). After heating the mixture on water bath at 70° to 80°C for 3 hours, ethanol was distilled off under a reduced pressure. To the residue was added water and the precipitated crystallines were separated by filtration, washed with water and dried to give the desired compound (1.8 g), which was recrystallized from ethanol. m.p. 180° to 183°C.

Workup

  1. temperatureAfter heating the mixture on water bath at 70° to 80°C for 3 hours
  2. distillationethanol was distilled off under a reduced pressure
  3. additionTo the residue was added water
  4. customthe precipitated crystallines were separated by filtration
  5. washwashed with water
  6. customdried

Sources & evidence

ORD record
ord-a2ac23eef9ef45b887bd5e5beeefa114
Source dataset
uspto-grants-1976_04
Patent number
US03948928

Reaction notes

Loading…