Hydroxyamine hydrochloride → HCID 73192201, compound

HRID 1108549Notes

Reaction equation

HRID 1108549 reaction equation
C([O-])(=O)C.[Na+].[CH3:6][C:7]1[CH:16]=[C:15]([CH3:17])[CH:14]=[C:13]2[C:8]=1[C:9](=O)[CH2:10][CH2:11][S:12]2.Cl.[NH2:20][OH:21]>O.C(O)C>[CH3:6][C:7]1[CH:16]=[C:15]([CH3:17])[CH:14]=[C:13]2[C:8]=1[C:9](=[N:20][OH:21])[CH2:10][CH2:11][S:12]2

Participants

6

Reactant 3

HCID 443297Hydroxyamine hydrochlorideHCID 517045Sodium AcetateHCID 15334888HCID 15334888, compound

Product 1

HCID 73192201HCID 73192201, compoundYield 69.5%

Reagents, catalysts & solvents 2

HCID 702EthanolSolventHCID 962WaterSolvent

Procedure

A suspension of 37.8 g of sodium acetate in water is added, at 50-60° C., to a suspension of 31.1 g (0.154 mol) of 5,7-dimethylthio-chroman-4-one and 18.5 g (0.261 mol) of hydroxylamine hydrochloride in 200 ml of ethanol. This mixture is subsequently refluxed for 30 minutes. After cooling, filtration with suction of the solid which has precipitated gives 22.2 g of 5,7-dimethylthiochroman-4-one oxime (66% of theory, purity approx. 95%) of melting point 170-174° C.

Workup

  1. temperatureThis mixture is subsequently refluxed for 30 minutes
  2. temperatureAfter cooling
  3. filtrationfiltration with suction of the solid which
  4. customhas precipitated

Sources & evidence

ORD record
ord-5c5e5b9bad72448cbe0d28df827e6962
Source dataset
uspto-grants-2000_05
Patent number
US06069114

Reaction notes

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