Hydroxylamine HCl → HCID 57353441, 화합물

HRID 1384770

반응식

HRID 1384770 반응식
[F:1][C:2]([F:13])([F:12])[C:3]([C:5]1[CH:10]=[CH:9][C:8]([CH3:11])=[CH:7][CH:6]=1)=O.[Cl-].[OH:15][NH3+:16].C([O-])(=O)C.[Na+]>C(O)C.O>[F:1][C:2]([F:13])([F:12])[C:3]([C:5]1[CH:10]=[CH:9][C:8]([CH3:11])=[CH:7][CH:6]=1)=[N:16][OH:15]

참가 물질

6

반응물 3

HCID 21645Hydroxylamine HClHCID 1362374-(Trifluoroacetyl)tolueneHCID 517045Sodium Acetate

생성물 1

HCID 57353441HCID 57353441, 화합물수율 73.4%

시약·촉매·용매 2

HCID 702Ethanol용매HCID 962Water용매

실험 절차

49.5 g (0.263 mol) of 2,2,2-trifluoro-1-(4-methylphenyl)-ethanone are dissolved in 250 ml of ethanol at 80° C. To the solution are added dropwise 19.2 g (0.276 mol) of hydroxylammonium chloride and 36.7 g (0.447 mol) of sodium acetate dissolved in 125 ml of water. The reaction mixture is refluxed for 3.5 hours. The mixture is poured into ice water, affording a white solid. The filtration yields 39.2 g of 2,2,2-trifluoro-1-(4-methylphenyl)-ethanone oxime as a white solid, mp. 54-68° C. The crude product is used in the next step without further purification.

후처리

  1. temperatureThe reaction mixture is refluxed for 3.5 hours
  2. customaffording a white solid
  3. filtrationThe filtration

출처 및 근거

ORD 기록
ord-4197629bd9334a8788f9666e2122225e
출처 데이터셋
uspto-grants-2001_07
특허 번호
US06261738B1

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