3,4,5-Trimethoxyhydrocinnamic acid → 5,6,7-Trimethoxy-1-indanone

HRID 1977998

반응식

HRID 1977998 반응식
[CH3:1][O:2][C:3]1[CH:4]=[C:5]([CH2:13][CH2:14][C:15]([OH:17])=O)[CH:6]=[C:7]([O:11][CH3:12])[C:8]=1[O:9][CH3:10]>O>[CH3:12][O:11][C:7]1[CH:6]=[C:5]2[C:4](=[C:3]([O:2][CH3:1])[C:8]=1[O:9][CH3:10])[C:15](=[O:17])[CH2:14][CH2:13]2

참가 물질

3

반응물 1

HCID 648603,4,5-Trimethoxyhydrocinnamic acid

생성물 1

HCID 6102105,6,7-Trimethoxy-1-indanone수율 89%

시약·촉매·용매 1

HCID 962Water용매

반응 조건

온도
80 °C

실험 절차

A mixture of 3-(3,4,5-trimethoxyphenyl)propionic acid (9.40 g, 39.1 mmol) and polyphosphoric acid (50 g) was stirred for 2 hours at 80° C. To the reaction mixture was added water, which was subjected to extraction with ethyl acetate. The extract solution was washed with brine, which was dried over anhydrous magnesium sulfate, followed by distilling off the solvent under reduced pressure. The residue was recrystallized from ethyl acetate/isopropyl ether to give 7.71 g (yield 89%) of the above-titled compound, m.p. 114-115° C.

후처리

  1. extractionwas subjected to extraction with ethyl acetate
  2. washThe extract solution was washed with brine, which
  3. dry with materialwas dried over anhydrous magnesium sulfate
  4. distillationby distilling off the solvent under reduced pressure
  5. customThe residue was recrystallized from ethyl acetate/isopropyl ether

출처 및 근거

ORD 기록
ord-be88cccdd0e04b61a3c603911ae5807d
출처 데이터셋
uspto-grants-2001_05
특허 번호
US06235789B1

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