Hydroxyamine hydrochloride → HCID 86631558, compound

HRID 885806Notes

Reaction equation

HRID 885806 reaction equation
[F:1][C:2]([F:19])([F:18])[CH:3]([NH:12][C:13](=[O:17])[CH:14]([CH3:16])[CH3:15])[C:4]1[CH:9]=[CH:8][C:7]([CH:10]=O)=[CH:6][CH:5]=1.Cl.[NH2:21][OH:22]>CO.O.C(OCC)(=O)C>[F:1][C:2]([F:19])([F:18])[CH:3]([NH:12][C:13](=[O:17])[CH:14]([CH3:16])[CH3:15])[C:4]1[CH:9]=[CH:8][C:7]([CH:10]=[N:21][OH:22])=[CH:6][CH:5]=1

Participants

6

Reactant 2

HCID 443297Hydroxyamine hydrochlorideHCID 86631559HCID 86631559, compound

Product 1

HCID 86631558HCID 86631558, compoundYield 118.5%

Reagents, catalysts & solvents 3

HCID 887MethanolSolventHCID 962WaterSolventHCID 8857Ethyl AcetateSolvent

Procedure

In a solution of 0.16 g of N-[2,2,2-trifluoro-1-(4-formylphenyl)ethyl]isobutyramide in 4.0 mL of methanol and 1.0 mL of water, 0.075 g of hydroxylamine hydrochloride was added, and stirred at room temperature for 1.5 hour. After the completion of the reaction, the reaction mixture was diluted with 20 mL of ethyl acetate, washed with water (10 mL×1), and the organic phase was dehydrated with and dried over saturated sodium chloride aqueous solution and anhydrous magnesium sulfate in that order, and the solvent was distilled off under reduced pressure to obtain 0.20 g of the aimed product as white crystal.

Workup

  1. customAfter the completion of the reaction
  2. washwashed with water (10 mL×1)
  3. dry with materialdried over saturated sodium chloride aqueous solution and anhydrous magnesium sulfate in that order
  4. distillationthe solvent was distilled off under reduced pressure

Sources & evidence

ORD record
ord-4d9ed518cbe94d19884c059ec748a931
Source dataset
uspto-grants-2012_08
Patent number
US08242283B2

Reaction notes

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