Water → 4-Methoxy-3-oxo-butyric acid-1-(3,3-dimethylcyclohexyl)-ethyl ester

HRID 1751172ノート

反応式

HRID 1751172 の反応式
[CH3:1][C:2]1([CH3:11])[CH2:7][CH2:6][CH2:5][CH:4]([CH:8]([OH:10])[CH3:9])[CH2:3]1.COC([CH2:16][CH2:17][C:18](=[O:22])[CH2:19][O:20][CH3:21])=O.CC[O-:25].[Na+].O>CO.C1(C)C=CC=CC=1>[CH3:11][C:2]1([CH3:1])[CH2:7][CH2:6][CH2:5][CH:4]([CH:8]([O:10][C:16](=[O:25])[CH2:17][C:18](=[O:22])[CH2:19][O:20][CH3:21])[CH3:9])[CH2:3]1

参加物

7

反応物 4

HCID 962WaterHCID 91338Cyclohexanemethanol, alpha,3,3-trimethyl-HCID 2723922Sodium ethoxideHCID 197524134-Methoxy-3-oxo-butanecarboxylic acid methyl ester

生成物 1

HCID 675154674-Methoxy-3-oxo-butyric acid-1-(3,3-dimethylcyclohexyl)-ethyl ester

試薬・触媒・溶媒 2

HCID 887Methanol溶媒2 回HCID 1140Toluene溶媒

実験手順

78 g (0.5 mol) of 1-(3,3-dimethyl-cyclohexyl)-ethanol, 80.3 g (0.55 mol) of 4-methoxy-3-oxo-butanecarboxylic acid methyl ester and 0.6 g sodium ethylate in 50 g methanol were placed in a 500-ml stirred vessel and boiled under reflux, distilling-off the methanol via a still head. Then 100 ml water and 100 ml toluene were added to the reaction solution at room temperature, the aqueous phase was separated, the organic phase was washed with water until neutral and concentrated by evaporation. The raw product (136 g) was fractionated on a 30-cm Vigreux column in vacuum.

後処理

  1. customthe aqueous phase was separated
  2. washthe organic phase was washed with water until neutral and
  3. concentrationconcentrated by evaporation

出典と根拠

ORDレコード
ord-3daca685e8bf4f87a8aeebc577f0d2f7
出典データセット
uspto-grants-2015_10
特許番号
US09157048B2

反応ノート

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