Hydroxylamine HCl → HCID 59115139, 화합물

HRID 1358159노트

반응식

HRID 1358159 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 54%

시약·촉매·용매 2

HCID 702Ethanol용매HCID 962Water용매

실험 절차

49.3 g (224 mmol) of 2,2,2-trifluoro-1-(4-methylsulfanyl-phenyl)-ethanone are dissolved in 250 ml of hot ethanol. To this solution is added dropwise a solution of hydroxylammonium chloride (16.3 g, 235 mmol) and sodium acetate (31.2 g, 381 mmol) in 125 ml of water, and the reaction solution is stirred under reflux for 6.5 hr. The reaction mixture was concentrated by rotary evaporation and poured into ice/water. The resulting yellow solid is filterd and washed with water. After drying under reduced pressure, recrystallization from hexane-ethyl acetate affords 28.4 g of white solid (54%). The structure is confirmed by the 1H-NMR spectrum (CDCl3), δ[ppm]:: d 2.51 (s, 3H), 7.31 (d, 2H), 7.49 (d, 2H), 8.80 (broad s, 1H).

후처리

  1. temperatureunder reflux for 6.5 hr
  2. concentrationThe reaction mixture was concentrated by rotary evaporation
  3. additionpoured into ice/water
  4. washwashed with water
  5. dry with materialAfter drying under reduced pressure, recrystallization from hexane-ethyl acetate

출처 및 근거

ORD 기록
ord-a16d994533da42cbab56bba4b6f2f8d7
출처 데이터셋
uspto-grants-2003_07
특허 번호
US06596445B1

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