3-(3,4,5-三甲氧基苯基)丙酸 → 5,6,7-Trimethoxy-1-indanone

HRID 1977998

反应方程式

HRID 1977998 反应方程式
[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

参与物

3

反应物 1

HCID 648603-(3,4,5-三甲氧基苯基)丙酸

产物 1

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

试剂、催化剂与溶剂 1

HCID 962聚[6-[4-(4-氰基苯基)苯氧基]己基甲基丙烯酸酯]溶剂

反应条件

温度
80 °C

实验过程

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.

后处理

  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

来源与证据

ORD记录
ord-be88cccdd0e04b61a3c603911ae5807d
来源数据集
uspto-grants-2001_05
专利号
US06235789B1

关联笔记

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