関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | Aluminum(III) Chloride | HCID 6451240 | — |
| 反応物 | 1,1-Dimethyl 2-ethenylcyclopropane-1,1-dicarboxylate | HCID 10464992 | — |
| 溶媒 | 1,2-Dimethoxyethane | HCID 8071 | — |
| 生成物 | 3-Chloro-5,5-dicarbomethoxy-1-pentene | HCID 23373951 | — |
反応手順
400 g of 1,2-dimethoxy ethane were introduced into a 1 liter glass flask equipped with a stirrer and a thermometer and admixed with 69 g of gaseous hydrogen chloride. 184.1 g of 1-vinyl-2,2-dicarbomethoxy cyclopropane (93.7% pure, 0.937 mol) and 0.65 g of aluminum chloride were then added to the contents, and the mixture was stirred. The temperature of the mixture rose to 40° C. The reaction was allowed to go to completion by letting the mixture stand overnight. After filtering off a slight turbidity, the reaction mixture was distilled in a 70 cm column. After collecting the 1,2-dimethoxy ethane which distilled over first and became available for reuse as a solvent in subsequent batches, the target product distilled over in pure form at 87° C./0.8 mbar.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US05569780 |
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| 出典データセット | uspto-grants-1996_10 |
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| ORD ID | ord-95caa92bd34847b1b7dec0e1f9ab1fb0 |
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| 出典メモ | uspto-grants-1996_10 |
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