関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Allyl chloride | HCID 7850 | — |
| 反応物 | Chlorobenzene | HCID 7964 | — |
| 反応物 | Malonic acid, disodium salt | HCID 8865 | — |
| 触媒 | Tetrabutylammonium Bromide | HCID 74236 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | Diallyl malonate | HCID 228227 | 16% |
反応手順
In an autoclave, 7.65 g (0.1 mol) of allyl chloride were added to a solution of 2.96 g (20 mmol) of disodium malonate and 0.64 g (2 mmol) of tetrabutylammonium bromide in 5 ml of water and 10 ml of chlorobenzene. The mixture was heated to 100° C. over a period of 30 minutes, with the pressure in the autoclave rising to 2.5 bar. After a reaction time of 3½ hours at 100° C., the mixture was cooled to room temperature and depressurized. The aqueous phase was extracted with tert-butyl methyl ether (2×5 ml). The combined organic phases were dried over sodium sulfate and analyzed by gas chromatography (internal standard: dimethyl succinate). The product yield was 16 percent.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US06350898B1 |
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| 出典データセット | uspto-grants-2002_02 |
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| ORD ID | ord-b57fe02393d84ac1b47f8c7cdcf0b734 |
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| 出典メモ | uspto-grants-2002_02 |
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