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3,4-Dimethoxy-β-methyl-2-propylbenzenebutanoic acid → HCID 10825371, 화합물

HRID 1955368
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인쇄 미리보기

반응식

HRID 1955368 반응식
[CH3:1][O:2][C:3]1[C:4]([CH2:18][CH2:19][CH3:20])=[C:5]([CH2:11][CH:12]([CH3:17])[CH2:13][C:14]([OH:16])=O)[CH:6]=[CH:7][C:8]=1[O:9][CH3:10]>C(Cl)Cl>[CH3:1][O:2][C:3]1[C:4]([CH2:18][CH2:19][CH3:20])=[C:5]2[C:6](=[CH:7][C:8]=1[O:9][CH3:10])[C:14](=[O:16])[CH2:13][CH:12]([CH3:17])[CH2:11]2
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

3

반응물 1

HCID 105168773,4-Dimethoxy-β-methyl-2-propylbenzenebutanoic acid

생성물 1

HCID 10825371HCID 10825371, 화합물수율 86%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

Compound 15b (7.0 g, 25 mmol) was added to 35 g of polyphosphoric ester in 100 mL of methylene chloride and refluxed for 1 h. The reaction mixture was poured onto ice, stirred, and extracted with ether. The ether was evaporated, and the residual oil was chromatographed on silica gel using ethyl acetate/hexane to give 5.63 g (21.5 mmol, 86% yield) of 16b as white crystals: 1H NMR:(ppm) 7.49 (s, 1H), 3.89 (s, 3H), 3.87 (s, 3H), 3.00-2.23 (mult, 7H), 1.50 (mult, 2H), 1.15 (d, 3H), 1.01 (t, 3H). Anal. (C16H22O3) C,H.

후처리

  1. temperaturerefluxed for 1 h
addition
The reaction mixture was poured onto ice
  • extractionextracted with ether
  • customThe ether was evaporated
  • customthe residual oil was chromatographed on silica gel
  • 출처 및 근거

    ORD 기록
    ord-7ab7e3fea90d4321893a98cbf4b489ca
    출처 데이터셋
    uspto-grants-2000_09
    DOI
    10.6084/m9.figshare.5104873.v1
    특허 번호
    US06124498

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