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3-(1,3-Dihydroxy-3-m-tolyl-propyl)-4-methoxy-benzoic acid methyl ester → 4-Methoxy-3-(3-m-tolyl-propyl)-benzoic acid methyl ester

HRID 521467
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인쇄 미리보기

반응식

HRID 521467 반응식
[CH3:1][O:2][C:3](=[O:24])[C:4]1[CH:9]=[CH:8][C:7]([O:10][CH3:11])=[C:6]([CH:12](O)[CH2:13][CH:14](O)[C:15]2[CH:16]=[C:17]([CH3:21])[CH:18]=[CH:19][CH:20]=2)[CH:5]=1.[H][H]>C(O)C.Cl.[Pd]>[CH3:1][O:2][C:3](=[O:24])[C:4]1[CH:9]=[CH:8][C:7]([O:10][CH3:11])=[C:6]([CH2:12][CH2:13][CH2:14][C:15]2[CH:16]=[C:17]([CH3:21])[CH:18]=[CH:19][CH:20]=2)[CH:5]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 2

HCID 670766153-(1,3-Dihydroxy-3-m-tolyl-propyl)-4-methoxy-benzoic acid methyl esterHCID 178418361HCID 178418361, 화합물

생성물 1

HCID 670764524-Methoxy-3-(3-m-tolyl-propyl)-benzoic acid methyl ester수율 63.2%

시약·촉매·용매 3

HCID 23938Palladium촉매HCID 313Hydrochloric Acid용매
HCID 702
Ethanol
용매

실험 절차

The compound of step 1 (140 mg, 0.424 mmol) was dissolved in ethanol (10 ml) and 12 N hydrochloric acid (0.2 ml), palladium on charcoal (10%) was added, and the mixture was hydrogenated at a hydrogen pressure of 6 bar at room temperature overnight. After filtration and evaporation, the residue was purified by silica gel chromatography (HEP/EA gradient) to give 80 mg of the title compound.

후처리

  1. filtrationAfter filtration and evaporation
  2. customthe residue was purified by silica gel chromatography (HEP/EA gradient)

출처 및 근거

ORD 기록
ord-52b72b9c2fc346e897684b1e723141d9
출처 데이터셋
uspto-grants-2016_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09328071B2

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