Hydroxyamine hydrochloride → HCID 86193537, compound

HRID 366636Notes

Reaction equation

HRID 366636 reaction equation
[Cl:1][C:2]([F:14])([F:13])[O:3][C:4]1[CH:5]=[C:6]([C:10](=O)[CH3:11])[CH:7]=[CH:8][CH:9]=1.Cl.[NH2:16][OH:17]>N1C=CC=CC=1>[Cl:1][C:2]([F:14])([F:13])[O:3][C:4]1[CH:5]=[C:6]([C:10](=[N:16][OH:17])[CH3:11])[CH:7]=[CH:8][CH:9]=1

Participants

4

Reactant 2

HCID 443297Hydroxyamine hydrochlorideHCID 23290025HCID 23290025, compound

Product 1

HCID 86193537HCID 86193537, compoundYield 106.4%

Reagents, catalysts & solvents 1

HCID 1049PyridineSolvent

Conditions

Temperature
50 °C

Procedure

A mixture of 3.3 g of 1-(3-(chloro-difluoro-methoxy)-phenyl)-ethanone, 1.4 g of hydroxylamine hydrochloride and 10 ml of pyridine is stirred at 50° C. for 2 hours. It is then poured into ice-water, extracted with diethyl ether and concentrated using a rotary evaporator, and any pyridine still present is removed azeotropically by means of toluene. Drying under reduced pressure at 60° C. yields 3.75 g of the desired oxime in the form of an oil.

Workup

  1. extractionextracted with diethyl ether
  2. concentrationconcentrated
  3. customa rotary evaporator
  4. customany pyridine still present is removed azeotropically by means of toluene
  5. customDrying under reduced pressure at 60° C.

Sources & evidence

ORD record
ord-4a4911aa029546128e02b6bf84631527
Source dataset
uspto-grants-2000_10
Patent number
US06130246

Reaction notes

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