5-Isopropenyl-2,4-dimethoxy-benzoic acid methyl ester → HCID 59263169, 화합물

HRID 425209노트

반응식

HRID 425209 반응식
[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]

참가 물질

4

반응물 1

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

생성물 1

HCID 59263169HCID 59263169, 화합물

시약·촉매·용매 2

HCID 23938Palladium촉매HCID 887Methanol용매

실험 절차

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.

후처리

  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)

출처 및 근거

ORD 기록
ord-42a5000e55b34284ab332e0e0e127df0
출처 데이터셋
uspto-grants-2012_01
특허 번호
US08106057B2

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