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Methyl methoxyacetate → Methoxyacetic acid-2-[1-(3,3-dimethyl-cyclohexyl)-ethoxy]-2-methyl-propyl ester
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Methyl methoxyacetate | HCID 80507 | — |
| 反応物 | Sodium Methoxide | HCID 10942334 | — |
| 反応物 | 2-[1-(3,3-Dimethyl-cyclohexyl)-ethoxy]-2-methyl-propan-1-ol | HCID 12022012 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 生成物 | Methoxyacetic acid-2-[1-(3,3-dimethyl-cyclohexyl)-ethoxy]-2-methyl-propyl ester | HCID 50996019 | — |
反応手順
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.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US09157048B2 |
| 出典データセット | uspto-grants-2015_10 |
| ORD ID | ord-e69ec2d88c9f4183b19ff6eada86696f |
| 出典メモ | uspto-grants-2015_10 |