Acetic Acid → Methyl 3-(3,5-dimethoxyphenyl)-2-(4-isopropyloxyphenyl)-3-oxopropionate

HRID 424030

反応式

HRID 424030 の反応式
[H-].[Na+].[CH3:3][O:4][C:5]1[CH:6]=[C:7]([CH:12]=[C:13]([O:15][CH3:16])[CH:14]=1)[C:8]([O:10]C)=O.[CH:17]([O:20][C:21]1[CH:26]=[CH:25][C:24]([CH2:27][C:28]([O:30][CH3:31])=[O:29])=[CH:23][CH:22]=1)([CH3:19])[CH3:18].C(O)(=O)C>C1(C)C=CC=CC=1.O>[CH3:16][O:15][C:13]1[CH:12]=[C:7]([C:8](=[O:10])[CH:27]([C:24]2[CH:25]=[CH:26][C:21]([O:20][CH:17]([CH3:19])[CH3:18])=[CH:22][CH:23]=2)[C:28]([O:30][CH3:31])=[O:29])[CH:6]=[C:5]([O:4][CH3:3])[CH:14]=1

参加物

7

反応物 4

HCID 176Acetic AcidHCID 24758Sodium hydrideHCID 75074Methyl 3,5-DimethoxybenzoateHCID 525538Methyl 2-(4-isopropoxyphenyl)acetate

生成物 1

HCID 66674372Methyl 3-(3,5-dimethoxyphenyl)-2-(4-isopropyloxyphenyl)-3-oxopropionate

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 1140Toluene溶媒4 回

反応条件

温度
2.5 °C

実験手順

14.4 g of 60% sodium hydride in mineral oil (0.36 mol) which are washed with 2 times 50 ml of toluene are introduced into a three-necked round-bottomed flask. 90 ml of toluene and 28.3 g of methyl 3,5-dimethoxybenzoate (0.144 mol) are then introduced. The mixture is brought to reflux and a solution of 30 g of methyl p-isopropyloxyphenylacetate (0.144 mol) dissolved in 95 ml of toluene is added over 10 h. The mixture is maintained at reflux for 2 h. It is cooled to a temperature of 0-5° C. and a solution of glacial acetic acid (22.5 g, i.e. 0.374 mol) in 25 ml of toluene is added slowly. Then, at ambient temperature, 135 ml of water are added slowly.

後処理

  1. additionare introduced into a three-necked round-bottomed flask
  2. temperatureto reflux
  3. additionis added over 10 h
  4. temperatureThe mixture is maintained
  5. temperatureat reflux for 2 h

出典と根拠

ORDレコード
ord-f134aec402f947f3b6994412ef96e865
出典データセット
uspto-grants-2012_01
特許番号
US08101804B2

関連ノート

読み込み中…