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

HRID 1751172Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1751172
[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

Komponenten

7

Edukt 4

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

Produkt 1

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

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 887MethanolLösungsmittel2×HCID 1140TolueneLösungsmittel

Versuchsvorschrift

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.

Aufarbeitung

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

Quellen und Nachweise

ORD-Eintrag
ord-3daca685e8bf4f87a8aeebc577f0d2f7
Quelldatensatz
uspto-grants-2015_10
Patentnummer
US09157048B2

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