反応式
[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]1参加物
5
実験手順
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.
後処理
- temperatureunder reflux
- distillationDuring this, methanol was distilled off via a still head
- additionThen 100 ml water and 100 ml toluene were added to the reaction solution at room temperature
- customthe aqueous phase was separated
- washthe organic phase was washed with water until neutral and
- concentrationconcentrated by evaporation
出典と根拠
- ORDレコード
- ord-e69ec2d88c9f4183b19ff6eada86696f
- 出典データセット
- uspto-grants-2015_10
- 特許番号
- US09157048B2
関連ノート
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