Hydroxyamine hydrochloride → HCID 87523172, compound

HRID 1477197Notes

Reaction equation

HRID 1477197 reaction equation
[CH3:1][N:2]([CH3:19])[C:3]1([C:12]2[CH:17]=[CH:16][CH:15]=[C:14]([F:18])[CH:13]=2)[CH2:8][CH2:7][C:6]([CH3:11])([CH:9]=O)[CH2:5][CH2:4]1.Cl.[NH2:21][OH:22]>C(O)C>[CH3:1][N:2]([CH3:19])[C:3]1([C:12]2[CH:17]=[CH:16][CH:15]=[C:14]([F:18])[CH:13]=2)[CH2:8][CH2:7][C:6]([CH3:11])([CH:9]=[N:21][OH:22])[CH2:5][CH2:4]1

Participants

4

Reactant 2

HCID 443297Hydroxyamine hydrochlorideHCID 87523600HCID 87523600, compound

Product 1

HCID 87523172HCID 87523172, compound

Reagents, catalysts & solvents 1

HCID 702EthanolSolvent

Procedure

A solution of the title compound of step 2 (1.38 g, 5.53 mmol) and hydroxylamine hydrochloride (576 mg, 8.3 mmol) in abs. ethanol (20 mL) were mixed with Amberlyst A 21 (3.9 g) and stirred for 16 h at RT. The ion exchanger was filtered off, the solution concentrated to low volume and the residue made alkaline with 1N NaOH. The aqueous phase was extracted with ethyl acetate, dried over Na2SO4 and concentrated to low volume in a vacuum.

Workup

  1. filtrationThe ion exchanger was filtered off
  2. concentrationthe solution concentrated to low volume
  3. extractionThe aqueous phase was extracted with ethyl acetate
  4. dry with materialdried over Na2SO4
  5. concentrationconcentrated to low volume in a vacuum

Sources & evidence

ORD record
ord-7f4ce4c3a3ac4f0e9a9cae2f8ec9ab3d
Source dataset
uspto-grants-2016_08
Patent number
US09403767B2

Reaction notes

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