Hydroxylamine HCl → HCID 59115139, 화합물

HRID 1636019노트

반응식

HRID 1636019 반응식
[F:1][C:2]([F:14])([F:13])[C:3]([C:5]1[CH:10]=[CH:9][C:8]([S:11][CH3:12])=[CH:7][CH:6]=1)=O.[Cl-].[OH:16][NH3+:17].C([O-])(=O)C.[Na+]>C(O)C.O>[F:1][C:2]([F:14])([F:13])[C:3]([C:5]1[CH:10]=[CH:9][C:8]([S:11][CH3:12])=[CH:7][CH:6]=1)=[N:17][OH:16]

참가 물질

6

반응물 3

HCID 21645Hydroxylamine HClHCID 517045Sodium AcetateHCID 27606164'-Thiomethyl-2,2,2-trifluoroacetophenone

생성물 1

HCID 59115139HCID 59115139, 화합물수율 97%

시약·촉매·용매 2

HCID 702Ethanol용매HCID 962Water용매

실험 절차

49.3 g (0.224 mol) of 2,2,2-trifluoro-1-(4-methylthiophenyl)-ethanone are dissolved in 250 ml of ethanol at 80° C. To the solution are added dropwise 16.3 g (0.235 mol) of hydroxylammonium chloride and 31.2 g (0.381 mol) of sodium acetate dissolved in 125 ml of water. The reaction mixture is refluxed for 6.5 hours, and poured into ice water. Filtration of the precipitate yields 51.1 g of 2,2,2-trifluoro-1-(4-methylthiophenyl)-ethanone oxime, as a yellow solid. The crude product is used in the next reaction step without further purification.

후처리

  1. temperatureThe reaction mixture is refluxed for 6.5 hours
  2. filtrationFiltration of the precipitate

출처 및 근거

ORD 기록
ord-67383eb2b278404b91e1fdf942f3759d
출처 데이터셋
uspto-grants-2003_01
특허 번호
US06512020B1

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