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Acetic Acid → Ethyl 3-bromo-6-hydroxy-2-methylbenzoate

HRID 365954
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HRID 365954 반응식
[Br:1]Br.C(O)(=O)C.[CH3:7][C:8]1[C:13]([C:14]([O:16][CH2:17][CH3:18])=[O:15])=[C:12]([OH:19])[CH:11]=[CH:10][CH:9]=1>O.C(OCC)(=O)C>[Br:1][C:9]1[CH:10]=[CH:11][C:12]([OH:19])=[C:13]([C:8]=1[CH3:7])[C:14]([O:16][CH2:17][CH3:18])=[O:15]
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참가 물질

6

반응물 3

HCID 176Acetic Acid2회HCID 24408BromineHCID 584222Ethyl 2-hydroxy-6-methylbenzoate

생성물 1

HCID 23293235Ethyl 3-bromo-6-hydroxy-2-methylbenzoate

시약·촉매·용매 2

HCID 962Water용매HCID 8857Ethyl Acetate용매

실험 절차

A mixture of bromine (5.05 ml, 0.099 mol) and acetic acid (15 ml) is added to a mixture of ethyl 6-methyl-2-hydroxybenzoate (17.05 g, 0.095 mol), and acetic acid (15 ml) at a temperature of 20° C. The reaction mixture is stirred at room temperature for 1 hour. The reaction mixture is diluted with water and ethyl acetate. The organic phase is washed with water twice, concentrated in vacuo and the residue is purified by flash chromatography (petrol ethers:ethyl acetate, 98:2 v/v) yielding the pure product as a yellow oil, 21.7 g, (88.2%).

후처리

  1. washThe organic phase is washed with water twice
  2. concentrationconcentrated in vacuo
  3. customthe residue is purified by flash chromatography (petrol ethers:ethyl acetate, 98:2 v/v)

출처 및 근거

ORD 기록
ord-a7b02d0bff1d45a7a3200b6dadfc077f
출처 데이터셋
uspto-grants-2000_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06127570

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