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

HRID 1977998

反応式

HRID 1977998 の反応式
[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

参加物

3

反応物 1

HCID 648603,4,5-Trimethoxyhydrocinnamic acid

生成物 1

HCID 6102105,6,7-Trimethoxy-1-indanone収率 89%

試薬・触媒・溶媒 1

HCID 962Water溶媒

反応条件

温度
80 °C

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-be88cccdd0e04b61a3c603911ae5807d
出典データセット
uspto-grants-2001_05
特許番号
US06235789B1

関連ノート

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