Diphenyl sulfide → 4-Chloro-2-(difluoromethoxy)phenol

HRID 2359304노트

반응식

HRID 2359304 반응식
[F:1][CH:2]([F:11])[O:3][C:4]1[CH:9]=[CH:8][CH:7]=[CH:6][C:5]=1[OH:10].[Cl-].[Cl-].[Cl-].[Al+3].S(C1C=CC=CC=1)C1C=CC=CC=1.S(Cl)([Cl:32])(=O)=O>ClCCl>[Cl:32][C:8]1[CH:7]=[CH:6][C:5]([OH:10])=[C:4]([O:3][CH:2]([F:11])[F:1])[CH:9]=1

참가 물질

6

반응물 4

HCID 8766Diphenyl sulfideHCID 24648Sulfuryl chlorideHCID 27741212-(Difluoromethoxy)phenolHCID 6451240Aluminum(III) Chloride

생성물 1

HCID 600510324-Chloro-2-(difluoromethoxy)phenol

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

To an ice cold suspension of 2-(difluoromethoxy)phenol (6.54 g, 0.00408 mol), aluminum trichloride (0.0544 g, 0.000408 mol) and 1,1′-thiodibenzene (0.068 mL, 0.000408 mol) was added sulfuryl dichloride (3.61 mL, 0.0449 mmol) dropwise. The reaction was allowed to warm to room temperature and stirred for 16 hours. The reaction was diluted in dichloromethane (10.0 mL) and purified using silica gel column chromatography eluting with 0-20% EtOAc in heptane. The title compound was isolated as a colourless oil (2.33 g, 0.01195 mol, 29%).

후처리

  1. custompurified
  2. washeluting with 0-20% EtOAc in heptane

출처 및 근거

ORD 기록
ord-d39ec5b0deb14b79b960b8f2276bf427
출처 데이터셋
uspto-grants-2014_04
특허 번호
US08685977B2

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