Hydroxyamine hydrochloride → HCID 86742024, compound

HRID 568665Notes

Reaction equation

HRID 568665 reaction equation
[F:1][C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][C:3]=1[C:8](=O)[C:9]1[CH:14]=[CH:13][C:12]([O:15][CH3:16])=[C:11]([Cl:17])[C:10]=1[Cl:18].Cl.[NH2:21][OH:22]>N1C=CC=CC=1>[Cl:18][C:10]1[C:11]([Cl:17])=[C:12]([O:15][CH3:16])[CH:13]=[CH:14][C:9]=1[C:8](=[N:21][OH:22])[C:3]1[CH:4]=[CH:5][CH:6]=[CH:7][C:2]=1[F:1]

Participants

4

Reactant 2

HCID 443297Hydroxyamine hydrochlorideHCID 13015710(2,3-Dichloro-4-methoxyphenyl)(2-fluorophenyl)methanone

Product 1

HCID 86742024HCID 86742024, compound

Reagents, catalysts & solvents 1

HCID 1049PyridineSolvent

Procedure

To a solution of 10 g (0.033 m) of 2'-fluoro-4-methoxy-2,3-dichlorobenzophenone of Example 1a in 100 ml of pyridine, 3.17 g of hydroxylamine HCl is added. The mixture is refluxed for about 64 hours. The pyridine is evaporated and the residue partitioned between 5% HCl and ethylacetate. The ethylacetate extract is washed with water, dried over Na2SO4 and evaporated to give 2,3-dichloro-4-methoxy-2'-fluorobenzophenone oxime, mp 195°-197° C.

Workup

  1. temperatureThe mixture is refluxed for about 64 hours
  2. customThe pyridine is evaporated
  3. customthe residue partitioned between 5% HCl and ethylacetate
  4. extractionThe ethylacetate extract
  5. washis washed with water
  6. dry with materialdried over Na2SO4
  7. customevaporated

Sources & evidence

ORD record
ord-7c9608c2624546a69fb130ca6aa01b2a
Source dataset
uspto-grants-1988_03
Patent number
US04728662

Reaction notes

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