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Chloroacetyl chloride → 2-Chloro-1-(2-fluoro-4,6-dimethoxyphenyl)ethan-1-one

HRID 411660
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HRID 411660 반응식
[CH3:1][O:2][C:3]1[CH:4]=[C:5]([F:11])[CH:6]=[C:7]([O:9][CH3:10])[CH:8]=1.[Cl:12][CH2:13][C:14](Cl)=[O:15].[Al+3].[Cl-].[Cl-].[Cl-]>ClC(Cl)C>[Cl:12][CH2:13][C:14]([C:6]1[C:7]([O:9][CH3:10])=[CH:8][C:3]([O:2][CH3:1])=[CH:4][C:5]=1[F:11])=[O:15]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 6577Chloroacetyl chlorideHCID 27742571-Fluoro-3,5-dimethoxybenzeneHCID 6451240Aluminum(III) Chloride

생성물 1

HCID 185413192-Chloro-1-(2-fluoro-4,6-dimethoxyphenyl)ethan-1-one

시약·촉매·용매 1

HCID 63651,1-Dichloroethane용매

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온도
0 °C

실험 절차

이 페이지에서참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

A solution consisting of 3,5-dimethoxy fluorobenzene 26 (5.0 g, 32 mmol) and chloroacetyl chloride (4.3 g, 38 mmol) in dichloroethane (100 mL) was cooled to 0° C. and treated with AlCl3 (5.1 g, 38 mmol). The reaction was allowed to rt and stirred for 1 h and then washed with 2N HCl aq, brine, dried over MgSO4, filtered, concentrated and chromatographed on silica gel (1:9 EtOAc/hexanes to 2:8 EtOAc/hexanes) to yiled th product 27 (1.2 g) as a white solid: Mp 93-96° C.

후처리

  1. customwas allowed to rt
  2. washwashed with 2N HCl aq, brine
  3. dry with materialdried over MgSO4
  4. filtrationfiltered
  5. concentrationconcentrated
  6. customchromatographed on silica gel (1:9 EtOAc/hexanes to 2:8 EtOAc/hexanes) to yiled th product 27 (1.2 g) as a white solid

출처 및 근거

ORD 기록
ord-c79011672fa04c26a0e262092493f46c
출처 데이터셋
uspto-grants-2003_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06559177B2

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