関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Lactonitrile | HCID 6572 | — |
| 反応物 | Diisopropylamine | HCID 7912 | — |
| 反応物 | Sulfuric acid magnesium salt (1:1) | HCID 24083 | — |
| 溶媒 | Diethyl Ether | HCID 3283 | — |
| 生成物 | 2-(Diisopropylamino)propionitrile | HCID 10997260 | 75% |
反応手順
Anhydrous magnesium sulfate (12.04 g, 0.1 mol) was added to diisopropylamine (12.14 g, 0.12 mol), followed by lactonitrile (7.73 g of 92% aqueous solution, 0.1 mol) added all at once with stirring. The reaction mixture spontaneously warmed up to 51° C. It was left overnight at room temperature. Diethyl ether (50 ml) was added, and magnesium sulfate was filtered off and washed with ether (50 ml). The product was isolated by distillation, 11.57 g, 75% yield, bp 49°-50° C./0.1 mm Hg. 1H NMR CDCl3 δ ppm, 1.02 (d, J=6.5 Hz, 6H, CH3), 1.17 (d, J=6.5 Hz, 6H, CH3), 1.41 (d, J=6.5 Hz, 3H, CH3, 3.21 (sep, J=6.5 Hz, 2H,=CH) , 3.89 (q, J=6.5 Hz, 1H, CH) .
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US05481038 |
|---|
| 出典データセット | uspto-grants-1996_01 |
|---|
| ORD ID | ord-c47826333e954a139ba74d6485ed7449 |
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| 出典メモ | uspto-grants-1996_01 |
|---|
