Hydroxyamine hydrochloride → HCID 73198224, compound

HRID 1596385Notes

Reaction equation

HRID 1596385 reaction equation
Cl.[NH2:2][OH:3].[CH:4]([C:6]1[CH2:7][O:8][C:9]2[CH:15]=[CH:14][C:13]([CH2:16][C:17]3[CH:18]=[N:19][CH:20]=[CH:21][CH:22]=3)=[CH:12][C:10]=2[CH:11]=1)=O>C(O)C.N1C=CC=CC=1>[CH:4](=[N:2][OH:3])[C:6]1[CH2:7][O:8][C:9]2[CH:15]=[CH:14][C:13]([CH2:16][C:17]3[CH:18]=[N:19][CH:20]=[CH:21][CH:22]=3)=[CH:12][C:10]=2[CH:11]=1

Participants

5

Reactant 2

HCID 443297Hydroxyamine hydrochlorideHCID 15463313HCID 15463313, compound

Product 1

HCID 73198224HCID 73198224, compoundYield 84.1%

Reagents, catalysts & solvents 2

HCID 702EthanolSolventHCID 1049PyridineSolvent

Procedure

Hydroxylamine hydrochloride was added to a mixed solution of 3.88 g (15.5 mmol) of 3-formyl-6-(3-pyridylmethyl)-2H-1-benzopyran in ethanol (35 ml) and pyridine (35 ml) at room temperature. The mixture was stirred for 2.5 hours was evaporated in vacuo and the residue was dispersed in chloroform-methanol (10:1). Then, after the organic layer was washed with water and brine, the solvent was evaporated in vacuo. The crystal precipitated during the evaporation of the solvent, was collected by filtration to obtain 3.46 g (yield=84.1%) of the desired compound.

Workup

  1. customwas evaporated in vacuo
  2. additionthe residue was dispersed in chloroform-methanol (10:1)
  3. washThen, after the organic layer was washed with water and brine
  4. customthe solvent was evaporated in vacuo
  5. customThe crystal precipitated during the evaporation of the solvent
  6. filtrationwas collected by filtration

Sources & evidence

ORD record
ord-572e1d4896fb4f80ab675959dfd97b73
Source dataset
uspto-grants-2001_09
Patent number
US06291482B1

Reaction notes

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