Hydroxylamine HCl → HCID 73455958, 화합물

HRID 1384773노트

반응식

HRID 1384773 반응식
[F:1][C:2]([F:14])([F:13])[C:3]([C:5]1[C:10]([CH3:11])=[CH:9][CH:8]=[CH:7][C:6]=1C)=O.[Cl-].[OH:16][NH3+:17].[C:18]([O-])(=O)C.[Na+]>C(O)C.O>[F:14][C:2]([F:1])([F:13])[C:3]([C:5]1[CH:6]=[CH:7][C:8]([CH3:18])=[CH:9][C:10]=1[CH3:11])=[N:17][OH:16]

참가 물질

6

반응물 3

HCID 21645Hydroxylamine HClHCID 517045Sodium AcetateHCID 186745371-(2,6-Dimethylphenyl)-2,2,2-trifluoroethan-1-one

생성물 1

HCID 73455958HCID 73455958, 화합물수율 88.4%

시약·촉매·용매 2

HCID 702Ethanol용매HCID 962Water용매

실험 절차

12.6 g (0.062 mol) of 2,2,2-trifluoro-1-(2,6-dimethylphenyl)-ethanone are dissolved in 30 ml of ethanol at 80° C. To the solution are added dropwise 4.6 g (0.066 mol) of hydroxylammonium chloride and 8.7 g (0.106 mol) of sodium acetate dissolved in 15 ml of water. The reaction mixture is refluxed overnight, affording white precipitation. The mixture is poured into ice water, and extracted with ethyl acetate. The organic phase is washed with water, NH4Cl aq, and brine, dried over MgSO4, and concentrated, yielding 11.9 g of crude 2,2,2-trifluoro-1-(2,4-dimethylphenyl)-ethanone oxime as a colorless liquid. The crude product is used in the next reaction step without further purification.

후처리

  1. temperatureThe reaction mixture is refluxed overnight
  2. customaffording white
  3. customprecipitation
  4. additionThe mixture is poured into ice water
  5. extractionextracted with ethyl acetate
  6. washThe organic phase is washed with water, NH4Cl aq, and brine
  7. dry with materialdried over MgSO4
  8. concentrationconcentrated

출처 및 근거

ORD 기록
ord-1f1d97fe663f446f9b309bcf526f6016
출처 데이터셋
uspto-grants-2001_07
특허 번호
US06261738B1

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