Hydroxyamine hydrochloride → HCID 136359213, compound

HRID 1156795Notes

Reaction equation

HRID 1156795 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][CH:9]=[CH:8][C:7]=1[F:12])=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][CH:9]=[CH:8][C:7]=1[F:12]

Participants

4

Reactant 2

HCID 443297Hydroxyamine hydrochlorideHCID 13015711HCID 13015711, compound

Product 1

HCID 136359213HCID 136359213, compoundYield 96%

Reagents, catalysts & solvents 1

HCID 1049PyridineSolvent

Procedure

A solution of 31.8 g (0.11 m) of 2,3-dichloro-4-hydroxy-2'-fluorobenzophenone of Example 2B and 15.29 g (0.22 m) of hydroxylamine hydrochloride in 150 ml of pyridine is refluxed 64 hours. The pyridine is evaporated in vacuo, 5% HCl added, extracted with ethyl acetate, dried (Na2SO4) and evaporated to give 32 g (96%) of 2,3-dichloro-4-hydroxy-2'-fluorobenzophenone oxime. An analytical sample is recrystallized from ethanol/H2O, m.p. 168°-175° C. TLC indicates the product is a mixture of isomers.

Workup

  1. customThe pyridine is evaporated in vacuo, 5% HCl
  2. additionadded
  3. extractionextracted with ethyl acetate
  4. dry with materialdried (Na2SO4)
  5. customevaporated

Sources & evidence

ORD record
ord-991f793faab846c297babf1bc7d82474
Source dataset
uspto-grants-1982_06
Patent number
US04337261

Reaction notes

Loading…