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

HRID 1003949ノート

反応式

HRID 1003949 の反応式
[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

参加物

5

反応物 1

HCID 98152983,5-Dimethoxystyrene

生成物 1

HCID 524877Benzene, 1,3-dimethoxy-5-ethyl収率 84.2%

試薬・触媒・溶媒 3

HCID 178418390HCID 178418390、化合物触媒HCID 887Methanol溶媒HCID 8857Ethyl Acetate溶媒

実験手順

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).

後処理

  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)

出典と根拠

ORDレコード
ord-2699772df4f44ca88778c0773a3eadb0
出典データセット
uspto-grants-2000_04
特許番号
US06048842

反応ノート

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