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3-Methoxybenzaldehyde → 2-Bromo-5-methoxybenzaldehyde

HRID 322983
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인쇄 미리보기

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HRID 322983 반응식
[CH3:1][O:2][C:3]1[CH:4]=[C:5]([CH:8]=[CH:9][CH:10]=1)[CH:6]=[O:7].[Br:11]Br>ClCCl>[Br:11][C:8]1[CH:9]=[CH:10][C:3]([O:2][CH3:1])=[CH:4][C:5]=1[CH:6]=[O:7]
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참가 물질

4

반응물 2

HCID 115693-MethoxybenzaldehydeHCID 24408Bromine

생성물 1

HCID 3444802-Bromo-5-methoxybenzaldehyde수율 105.2%

시약·촉매·용매 1

HCID 6344Dichloromethane용매2회

실험 절차

A stirred solution of 3-methoxybenzaldehyde (27.23 g) in dichloromethane (150 mL) at 0° C. is treated with a solution of bromine (32 g) in dry dichloromethane (50 mL) over 30 minutes. The reaction mixture is stirred at room temperature for 4 hours, combined with a previous preparation carried out on the same scale, and washed with saturated sodium metabisulphite solution (400 mL), with water (400 mL), brine (400 mL) and dried over magnesium sulphate. Evaporation and recrystallisation of the residue from petroleum ether (b.p. 40-60° C.) gives 2-bromo-5-methoxybenzaldehyde (45.25 g) as a white solid, m.p. 73-74° C.

후처리

  1. customcombined with a previous preparation
  2. washwashed with saturated sodium metabisulphite solution (400 mL), with water (400 mL), brine (400 mL)
  3. dry with materialdried over magnesium sulphate
  4. customEvaporation and recrystallisation of the residue from petroleum ether (b.p. 40-60° C.)

출처 및 근거

ORD 기록
ord-c49ce4cdfafe48bd8e0ee62d812a027f
출처 데이터셋
uspto-grants-2001_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06211234B1

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