Hydroxylamine HCl → HCID 137182986, compound

HRID 428812Notes

Reaction equation

HRID 428812 reaction equation
[CH2:1]([O:3][N:4]=[C:5]([C:9]1[CH:14]=[CH:13][C:12]([O:15][CH2:16][Si:17]([CH3:26])([CH3:25])[C:18]2[CH:23]=[CH:22][C:21]([F:24])=[CH:20][CH:19]=2)=[CH:11][CH:10]=1)[C:6](=O)[CH3:7])[CH3:2].[Cl-].[OH:28][NH3+:29]>N1C=CC=CC=1>[CH2:1]([O:3][N:4]=[C:5]([C:9]1[CH:14]=[CH:13][C:12]([O:15][CH2:16][Si:17]([CH3:26])([CH3:25])[C:18]2[CH:23]=[CH:22][C:21]([F:24])=[CH:20][CH:19]=2)=[CH:11][CH:10]=1)[C:6](=[N:29][OH:28])[CH3:7])[CH3:2]

Participants

4

Reactant 2

HCID 21645Hydroxylamine HClHCID 131722973HCID 131722973, compound

Product 1

HCID 137182986HCID 137182986, compound

Reagents, catalysts & solvents 1

HCID 1049PyridineSolvent

Procedure

14.3 g of 1-(4-[{dimethyl-(4-fluorophenyl)-silyl}methoxy]phenyl)-propane-1,2-dione-1-ethyl-oxime in 50 ml of pyridine are stirred with 3.5 g of hydroxylammonium chloride for 2 hours at 70° C. The reaction mixture is concentrated in vacuo and ethyl acetate is added to the residue; the organic phase is washed with water and saturated sodium chloride solution and dried over sodium sulfate; the solvent is evaporated off. Recrystallisation from hexane yields the title product having a melting point of 100-102° C.

Workup

  1. concentrationThe reaction mixture is concentrated in vacuo and ethyl acetate
  2. additionis added to the residue
  3. washthe organic phase is washed with water and saturated sodium chloride solution
  4. dry with materialdried over sodium sulfate
  5. customthe solvent is evaporated off
  6. customRecrystallisation from hexane

Sources & evidence

ORD record
ord-69ce8d75f9b54702b13e360c36b05c07
Source dataset
uspto-grants-2001_11
Patent number
US06313344B1

Reaction notes

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