5-Isopropenyl-2,4-dimethoxy-benzoic acid methyl ester → HCID 59263169、化合物

HRID 334944

反応式

HRID 334944 の反応式
[CH3:1][O:2][C:3](=[O:17])[C:4]1[CH:9]=[C:8]([C:10]([CH3:12])=[CH2:11])[C:7]([O:13][CH3:14])=[CH:6][C:5]=1[O:15][CH3:16]>CO.[Pd]>[CH3:1][O:2][C:3](=[O:17])[C:4]1[CH:9]=[C:8]([CH:10]([CH3:12])[CH3:11])[C:7]([O:13][CH3:14])=[CH:6][C:5]=1[O:15][CH3:16]

参加物

4

反応物 1

HCID 592631485-Isopropenyl-2,4-dimethoxy-benzoic acid methyl ester

生成物 1

HCID 59263169HCID 59263169、化合物

試薬・触媒・溶媒 2

HCID 23938Palladium触媒HCID 887Methanol溶媒

実験手順

A solution of 5-isopropenyl-2,4-dimethoxy-benzoic acid methyl ester (6.0 g, 25.4 mmol) in MeOH (85 ml) was shaken with 10% Pd/C under an atmosphere of H2 at room temperature for 3 hours. The catalyst was filtered through GF/A paper but a little fine powder passed through. The filtrate was passed through a small pad of silica and evaporated to dryness to yield a colourless solid. The product was purified by flash column chromatography (DCM:Petrol gradient elution) to yield 5-isopropyl-2,4-dimethoxy-benzoic acid methyl ester a colourless solid (5.5 g). 1H NMR (Me-d3-OD) 7.68 (1H, s), 6.64 (1H, s), 3.94 (3H, s), 3.91 (3H, s), 3.84 (3H, s), 3.23 (1H, sept), 1.20 (6H, d). MS: [M+H]+ 239.

後処理

  1. filtrationThe catalyst was filtered through GF/A paper
  2. customevaporated to dryness
  3. customto yield a colourless solid
  4. customThe product was purified by flash column chromatography (DCM:Petrol gradient elution)

出典と根拠

ORDレコード
ord-d2e04d6b7760427eb32c1fbab7491cde
出典データセット
uspto-grants-2014_11
特許番号
US08883790B2

関連ノート

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