Methyl iodide → 4-Bromo-1-methanesulfonyl-2-(trifluoromethoxy)benzene

HRID 2103639노트

반응식

HRID 2103639 반응식
[Br:1][C:2]1[CH:7]=[CH:6][C:5](S)=[C:4]([O:9][C:10]([F:13])([F:12])[F:11])[CH:3]=1.IC.[C:16](=O)([O-])[O-].[K+].[K+].BrC1C=CC(SC)=C(OC(F)(F)F)C=1.O[O:37][S:38]([O-:40])=O.[K+]>CC(C)=O>[Br:1][C:2]1[CH:7]=[CH:6][C:5]([S:38]([CH3:16])(=[O:40])=[O:37])=[C:4]([O:9][C:10]([F:13])([F:12])[F:11])[CH:3]=1

참가 물질

7

반응물 5

HCID 6328Methyl iodideHCID 11430Potassium CarbonateHCID 27364254-Bromo-2-(trifluoromethoxy)thiophenolHCID 187114734-Bromo-2-(trifluoromethoxy)thioanisoleHCID 23707502Potassium hydroxy sulfite3회

생성물 1

HCID 534180354-Bromo-1-methanesulfonyl-2-(trifluoromethoxy)benzene

시약·촉매·용매 1

HCID 180Acetone용매

실험 절차

Following the method of example 9a, reaction of 4-bromo-2-trifluoromethoxy-benzenethiol (1.0 g, 3.48 mmol) with iodomethane (0.238 mL, 3.82 mmol) and potassium carbonate (0.528 g, 3.82 mmol) in 13 mL acetone, followed by oxidation as described in example 39c, using 4-bromo-1-methylsulfanyl-2-trifluoromethoxy-benzene (0.78 g, 2.72 mmol) and oxone® (2.17 g, 3.54 mmol), stirring over night at r.t., addition of oxone® (0.84 g, 1.37 mmol), stirring over night at r.t., addition of oxone® (0.84 g, 1.37 mmol) and stirring over three days at r.t. affords the title compound without further chromatography as a white solid (0.81 g). MS (m/e): 320 (M+H).

후처리

  1. stirringstirring over night at r.t.
  2. stirringstirring over three days at r.t.

출처 및 근거

ORD 기록
ord-5b68ea12096e497bbccaaf09405d7928
출처 데이터셋
uspto-grants-2009_08
특허 번호
US07576108B2

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