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

HRID 1751172

반응식

HRID 1751172 반응식
[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

참가 물질

7

반응물 4

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

생성물 1

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

시약·촉매·용매 2

HCID 887Methanol용매2회HCID 1140Toluene용매

실험 절차

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.

후처리

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

출처 및 근거

ORD 기록
ord-3daca685e8bf4f87a8aeebc577f0d2f7
출처 데이터셋
uspto-grants-2015_10
특허 번호
US09157048B2

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