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Dimethylacetylene → Dimethyl 2,3-dimethyl-2-cyclopropene-1,1-dicarboxylate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Dimethylacetylene | HCID 10419 | — |
| 反応物 | 2-Diazonio-1,3-dimethoxy-3-oxoprop-1-en-1-olate | HCID 547673 | — |
| 触媒 | Mercury | HCID 23931 | — |
| 溶媒 | Hexafluorobenzene | HCID 9805 | — |
| 生成物 | Dimethyl 2,3-dimethyl-2-cyclopropene-1,1-dicarboxylate | HCID 19096835 | 46.2% |
反応手順
A nitrogen-degassed solution of 37.5 grams (0.69 mole) of 2-butyne and 20.0 grams (0.13 mole) of dimethyl diazomalonate in approximately 325 grams of hexafluorobenzene was photolyzed for approximately 100 hours, at 0° C.-5° C., employing a 100-watt Hanovia mercury lamp in a manner similar to that described in Example XCVI Part A. Similar workup of the reaction mixture afforded 10.8 grams (0.06 mole) of dimethyl 2,3-dimethyl-2-cyclopropene-1,1-dicarboxylate. NMR analysis of the product indicated the following:
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05123951 |
| 出典データセット | uspto-grants-1992_06 |
| ORD ID | ord-45b0c1b72dcb41cf8cec21d7fa3430ea |
| 出典メモ | uspto-grants-1992_06 |