関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | Sodium Iodide | HCID 5238 | — |
| 反応物 | Sodium acrylate | HCID 4068533 | — |
| 反応物 | 4'-Pentyl-bicyclohexyl-4-carboxylic acid 6-(2-methyl-acryloyloxy)-hexyl ester | HCID 59289040 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | 4'-Propyl-bicyclohexyl-4-carboxylic acid 3-acryloyloxy-propyl ester | HCID 59289070 | — |
反応手順
A mixture of sodium acrylate (2.5 g, 13.4 mmol), 4′-propyl-bicyclohexyl-4-carboxylic acid 3-bromo-propyl ester (synthesis described for preferred example 1) (5.0 g, 13.4 mmol) and sodium iodide (2.5 g, 16.7 mmol) in dimethylformamide (150 ml) is stirred at 130° C. overnight. The mixture is cooled to room temperature, poured into water, and this is extracted twice with diethyl ether. The ethereal solution is washed with water and then dried over sodium sulphate. The solution is evaporated to dryness and purified by flash column chromatography using DCM/petrol (1/1) as eluant to give upon evaporation of the appropriate fractions a colourless oil.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08372307B2 |
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| 出典データセット | uspto-grants-2013_02 |
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| ORD ID | ord-3352ca3e5f3a43e796f555dd60c1a09a |
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| 出典メモ | uspto-grants-2013_02 |
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