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Acetic Acid → (3,3-Dimethylbutan-2-ylidene)propanedinitrile
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Acetic Acid | HCID 176 | — |
| 反応物 | Pinacolone | HCID 6416 | — |
| 反応物 | Malononitrile | HCID 8010 | — |
| 反応物 | Ammonium Acetate | HCID 517165 | — |
| 溶媒 | Toluene | HCID 1140 | — |
| 生成物 | (3,3-Dimethylbutan-2-ylidene)propanedinitrile | HCID 534326 | 68.4% |
反応手順
A solution of 9.9 g of malononitrile, 26.25 g of 3,3-dimethyl-2-butanone, 1.45 g of ammonium acetate and 2.25 g of acetic acid dissolved in 100 ml of toluene was refluxed for about 16 hours with the aid of a Dean-Stark Trap. The reaction mixture was diluted with 120 ml of toluene and washed with 200 ml water. The organic phase was collected, dried over anhydrous magnesium sulfate, filtered and concentrated under vacuum. The resulting residue was distilled under vacuum to afford 15.2 g of 2-(1,1-dimethylethyl)-1,1-dicyano-1-propene as an oil. Yield 68%.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04643758 |
| 出典データセット | uspto-grants-1987_02 |
| ORD ID | ord-aa5428eb78a445e4ae7e7564a987dd8c |
| 出典メモ | uspto-grants-1987_02 |