Water → 3-Oxo-hexanoic acid-1-(3,3-dimethyl-cyclohexyl)-ethyl ester

HRID 1751173노트

반응식

HRID 1751173 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.C(O[C:15]([CH2:17][CH2:18][C:19](=[O:23])[CH2:20][CH2:21]C)=O)C.CC[O-:26].[Na+].O>C(O)C.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:21](=[O:26])[CH2:20][C:19](=[O:23])[CH2:18][CH2:17][CH3:15])[CH3:9])[CH2:3]1

참가 물질

7

반응물 4

HCID 962WaterHCID 91338Cyclohexanemethanol, alpha,3,3-trimethyl-HCID 2723922Sodium ethoxideHCID 12271529Ethyl 4-oxoheptanoate

생성물 1

HCID 675167043-Oxo-hexanoic acid-1-(3,3-dimethyl-cyclohexyl)-ethyl ester

시약·촉매·용매 2

HCID 702Ethanol용매2회HCID 1140Toluene용매

실험 절차

78 g (0.5 mol) of 1-(3,3-dimethyl-cyclohexyl)-ethanol, 86.9 g (0.55 mol) of 3-oxo-hexanecarboxylic acid ethyl ester and 0.6 g sodium ethylate in 50 g ethanol were placed in a 500-ml stirred vessel and boiled under reflux, distilling-off the ethanol 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 (139 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-7b5c2e79de0c47b8ba2d40445083f433
출처 데이터셋
uspto-grants-2015_10
특허 번호
US09157048B2

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