Hydroxyamine hydrochloride → HCID 87523172, compound

HRID 76937Notes

Reaction equation

HRID 76937 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-1c8c36515e974ea28a8b6fa674685889
Source dataset
uspto-grants-2014_09
Patent number
US08835689B2

Reaction notes

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