Methyl methoxyacetate → Methoxyacetic acid-2-[1-(3,3-dimethyl-cyclohexyl)-ethoxy]-2-methyl-propyl ester

HRID 1751170

반응식

HRID 1751170 반응식
[CH3:1][C:2]1([CH3:16])[CH2:7][CH2:6][CH2:5][CH:4]([CH:8]([O:10][C:11]([CH3:15])([CH3:14])[CH2:12][OH:13])[CH3:9])[CH2:3]1.[CH3:17][O:18][C:19](=O)[CH2:20][O:21]C.C[O-].[Na+]>CO>[CH3:16][C:2]1([CH3:1])[CH2:7][CH2:6][CH2:5][CH:4]([CH:8]([O:10][C:11]([CH3:15])([CH3:14])[CH2:12][O:13][C:20](=[O:21])[CH2:19][O:18][CH3:17])[CH3:9])[CH2:3]1

참가 물질

5

반응물 3

HCID 80507Methyl methoxyacetateHCID 10942334Sodium MethoxideHCID 120220122-[1-(3,3-Dimethyl-cyclohexyl)-ethoxy]-2-methyl-propan-1-ol

생성물 1

HCID 50996019Methoxyacetic acid-2-[1-(3,3-dimethyl-cyclohexyl)-ethoxy]-2-methyl-propyl ester

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

57 g (0.25 mol) of 2-[1-(3,3-dimethyl-cyclohexyl)-ethoxy]-2-methyl-propan-1-ol, 41.6 g (0.4 mol) of methoxyacetic acid methyl ester and 0.3 g of sodium methylate in 50 g methanol were placed in a 250-ml stirred vessel and were boiled under reflux. During this, methanol was distilled off 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 (81 g) was fractionated on a 30-cm Vigreux column in vacuum.

후처리

  1. temperatureunder reflux
  2. distillationDuring this, methanol was distilled off via a still head
  3. additionThen 100 ml water and 100 ml toluene were added to the reaction solution at room temperature
  4. customthe aqueous phase was separated
  5. washthe organic phase was washed with water until neutral and
  6. concentrationconcentrated by evaporation

출처 및 근거

ORD 기록
ord-e69ec2d88c9f4183b19ff6eada86696f
출처 데이터셋
uspto-grants-2015_10
특허 번호
US09157048B2

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