3,5-Dimethoxystyrene → Benzene, 1,3-dimethoxy-5-ethyl

HRID 1003949노트

반응식

HRID 1003949 반응식
[CH3:1][O:2][C:3]1[CH:4]=[C:5]([CH:8]=[C:9]([O:11][CH3:12])[CH:10]=1)[CH:6]=[CH2:7]>CO.C(OCC)(=O)C.[C].[Pd]>[CH3:12][O:11][C:9]1[CH:8]=[C:5]([CH2:6][CH3:7])[CH:4]=[C:3]([O:2][CH3:1])[CH:10]=1

참가 물질

5

반응물 1

HCID 98152983,5-Dimethoxystyrene

생성물 1

HCID 524877Benzene, 1,3-dimethoxy-5-ethyl수율 84.2%

시약·촉매·용매 3

HCID 178418390HCID 178418390, 화합물촉매HCID 887Methanol용매HCID 8857Ethyl Acetate용매

실험 절차

3,5-Dimethoxystyrene (8.29 g) is dissolved in a mixture of methanol (70 ml) and ethyl acetate (10 ml), and the mixture is subjected to catalytic hydrogenation with using 10% palladium-carbon (51.4% aqueous, 1.2 g) under atmospheric pressure. One hour thereafter, the catalyst is removed by filtration, and the filtrate is concentrated under reduced pressure. The residue is purified by silica gel column chromatography (solvent; hexane/ethyl acetate) to give 1,3-dimethoxy-5-ethylbenzene (7.07 g).

후처리

  1. customOne hour thereafter, the catalyst is removed by filtration
  2. concentrationthe filtrate is concentrated under reduced pressure
  3. customThe residue is purified by silica gel column chromatography (solvent; hexane/ethyl acetate)

출처 및 근거

ORD 기록
ord-2699772df4f44ca88778c0773a3eadb0
출처 데이터셋
uspto-grants-2000_04
특허 번호
US06048842

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