関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Allyl Alcohol | HCID 7858 | — |
| 反応物 | (Diethoxyphosphinyl)acetic acid | HCID 36704 | — |
| 反応物 | N-(3-methylaminopropyl)-N'-ethylcarbodiimide hydrochloride | HCID 9794023 | — |
| 触媒 | 4-(Dimethylamino)pyridine | HCID 14284 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | Allyl P,P-diethylphosphonoacetate | HCID 4583084 | 82.2% |
反応手順
29.2 g of the diethylphosphonoacetic acid thus obtained was dissolved in 350 me of methylene chloride, and 17.8 g of allyl alcohol, 1.92 g of 4-dimethylaminopyridine and 29.0 g of 1-ethyl-3-(3-methylaminopropyl)carbodiimide hydrochloride were added thereto with stirring under cooling with ice. The mixture was stirred at room temperature overnight. The reaction solution was evaporated under reduced pressure. The residue was dissolved in ethyl acetate, then sequentially washed with 1N hydrochloric acid, water, a saturated sodium hydrogencarbonate aqueous solution and a saturated sodium chloride aqueous solution, and dried over anhydrous magnesium sulfate. The drying agent was separated by filtration, and then the solvent was distilled off under reduced pressure to obtain 28.9 g of allyl diethylphosphonoacetate.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US05616803 |
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| 出典データセット | uspto-grants-1997_04 |
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| ORD ID | ord-d728077f295740f79612ef0dd40891fd |
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| 出典メモ | uspto-grants-1997_04 |
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