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2-Fluoroanisole → 4-(3-Fluoro-4-methoxy-benzoyl)-benzoic acid methyl ester

HRID 229248
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HRID 229248 반응식
[Al+3].[Cl-].[Cl-].[Cl-].[CH3:5][O:6][C:7](=[O:17])[C:8]1[CH:13]=[CH:12][C:11]([C:14](Cl)=[O:15])=[CH:10][CH:9]=1.[F:18][C:19]1[CH:24]=[CH:23][CH:22]=[CH:21][C:20]=1[O:25][CH3:26]>ClCCl>[CH3:5][O:6][C:7](=[O:17])[C:8]1[CH:13]=[CH:12][C:11]([C:14](=[O:15])[C:23]2[CH:22]=[CH:21][C:20]([O:25][CH3:26])=[C:19]([F:18])[CH:24]=2)=[CH:10][CH:9]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 675762-FluoroanisoleHCID 81850Methyl 4-(chlorocarbonyl)benzoateHCID 6451240Aluminum(III) Chloride

생성물 1

HCID 686545474-(3-Fluoro-4-methoxy-benzoyl)-benzoic acid methyl ester수율 17.2%

시약·촉매·용매 1

HCID 6344Dichloromethane용매3회

실험 절차

To an ice-cooled slurry of AlCl3 (2.01 g, 15.1 mmol) in dichloromethane (10 mL) was slowly added 4-chlorocarbonyl-benzoic acid methyl ester (2 g, 10.1 mmol) in dichloromethane (5 mL). The reaction mixture was stirred for 20 min in the ice bath then 2-fluoroanisole (1.4 mL, 12.1 mmol) in dichloromethane (5 mL) was added. The reaction mixture was stirred at room temperature for 20 h. The reaction mixture was poured into ice cold 1 N HCl (10 mL) and the mixture was stirred for 15 min. The reaction mixture was transferred to a separatory funnel and the layers were separated. The aqueous layer was extracted with dichloromethane and the organic extracts were combined, washed with brine, dried over Na2SO4, filtered and concentrated. The crude solid was triturated with hot hexanes, filtered and washed with hexanes to give 0.5 g (17%) of compound 173 as a white powder. 1H NMR (400 MHz, DMSO-d6): δ 3.89 (s, 3H), 3.94 (s, 3H), 7.32 (t, J=8.5 Hz, 1H), 7.57 (d, J=8.8 Hz, 1H), 7.59-7.63 (m, 1H), 7.81 (d, J=8.2 Hz, 2H), 8.04 (s, 1H), 8.10 (d, J=8.3 Hz, 2H).

후처리

  1. stirringthe mixture was stirred for 15 min
  2. customThe reaction mixture was transferred to a separatory funnel
  3. customthe layers were separated
  4. extractionThe aqueous layer was extracted with dichloromethane
  5. washwashed with brine
  6. dry with materialdried over Na2SO4
  7. filtrationfiltered
  8. concentrationconcentrated
  9. customThe crude solid was triturated with hot hexanes
  10. filtrationfiltered
  11. washwashed with hexanes

출처 및 근거

ORD 기록
ord-b64d8e49f5674c098f2dbc283974b5ee
출처 데이터셋
uspto-grants-2009_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07560589B2

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