Hydroxyamine hydrochloride → HCID 136393679, compound

HRID 652846Notes

Reaction equation

HRID 652846 reaction equation
[Cl:1][C:2]1[C:16]([Cl:17])=[C:15]([OH:18])[CH:14]=[CH:13][C:3]=1[C:4]([C:6]1[CH:11]=[CH:10][C:9]([CH3:12])=[CH:8][CH:7]=1)=O.Cl.[NH2:20][OH:21]>N1C=CC=CC=1>[Cl:1][C:2]1[C:16]([Cl:17])=[C:15]([OH:18])[CH:14]=[CH:13][C:3]=1[C:4](=[N:20][OH:21])[C:6]1[CH:11]=[CH:10][C:9]([CH3:12])=[CH:8][CH:7]=1

Participants

4

Reactant 2

HCID 443297Hydroxyamine hydrochlorideHCID 20150492HCID 20150492, compound

Product 1

HCID 136393679HCID 136393679, compound

Reagents, catalysts & solvents 1

HCID 1049PyridineSolvent

Procedure

A mixture of 2,3-dichloro-4-hydroxy-4'-methylbenzophenone and 12.5 g of hydroxylamine hydrochloride in 200 ml of pyridine is refluxed for 2 hours. Thereafter the pyridine is evaporated off under vacuum and the residue is partitioned between ethyl acetate and 5% hydrochloric acid. The ethyl acetate extract is, successively, washed with water, dried and concentrated to dryness leaving 2,3-dichloro-4-hydroxy-4'-methylbenzophenone oxime.

Workup

  1. temperatureis refluxed for 2 hours
  2. customThereafter the pyridine is evaporated off under vacuum
  3. customthe residue is partitioned between ethyl acetate and 5% hydrochloric acid
  4. extractionThe ethyl acetate extract
  5. washsuccessively, washed with water
  6. customdried
  7. concentrationconcentrated to dryness

Sources & evidence

ORD record
ord-fc28a74fb7444622a0f1eb64b757401e
Source dataset
uspto-grants-1987_06
Patent number
US04673746

Reaction notes

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