4'-Fluoroacetophenone → 1-[4-(4-Chloro-3-trifluoromethylphenoxy)-phenyl]-ethanone

HRID 474613

반응식

HRID 474613 반응식
[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([OH:8])=[CH:4][C:3]=1[C:9]([F:12])([F:11])[F:10].F[C:14]1[CH:19]=[CH:18][C:17]([C:20](=[O:22])[CH3:21])=[CH:16][CH:15]=1.C([O-])([O-])=O.[K+].[K+]>CN(C=O)C.CC(=O)OCC>[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([O:8][C:14]2[CH:19]=[CH:18][C:17]([C:20](=[O:22])[CH3:21])=[CH:16][CH:15]=2)=[CH:4][C:3]=1[C:9]([F:10])([F:11])[F:12]

참가 물질

6

반응물 3

HCID 98284'-FluoroacetophenoneHCID 11430Potassium CarbonateHCID 805204-Chloro-3-(trifluoromethyl)phenol

생성물 1

HCID 677750201-[4-(4-Chloro-3-trifluoromethylphenoxy)-phenyl]-ethanone수율 97.4%

시약·촉매·용매 2

HCID 6228Dimethylformamide용매HCID 8857Ethyl Acetate용매

반응 조건

온도
145 °C

실험 절차

A mixture of 4-chloro-3-(trifluoromethyl)phenol (2 g, 10.18 mmol), 1-(4-fluorophenyl) ethanone (1.406 g) and K2CO3 (2.3 g, 16.64 mmol) in DMF (18 mL) was heated with a microwave condition at 145° C. for 4 h. The solution was diluted with EA and washed with water twice, dried over Na2SO4 and concentrated in vacuo to afford the title compound (3.12 g, 97% yield) as a brown oil. LCMS: rt=3.83 min, [M+H+]=315

후처리

  1. washwashed with water twice
  2. dry with materialdried over Na2SO4
  3. concentrationconcentrated in vacuo

출처 및 근거

ORD 기록
ord-d136af2ecdab44e1b33ffca4552371bf
출처 데이터셋
uspto-grants-2014_01
특허 번호
US08637536B2

연결된 노트

불러오는 중…