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Carbon Dioxide → 2-[(4-t-Butyl-1-piperidyl)methyl]propenenitrile
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Carbon Dioxide | HCID 280 | — |
| 反応物 | Formaldehyde | HCID 712 | — |
| 反応物 | Cyanoacetic acid | HCID 9740 | — |
| 反応物 | Piperidine, 4-(1,1-dimethylethyl)- | HCID 74661 | — |
| 溶媒 | Diethyl Ether | HCID 3283 | — |
| 溶媒 | 1,4-Dioxane | HCID 31275 | — |
| 生成物 | 2-[(4-t-Butyl-1-piperidyl)methyl]propenenitrile | HCID 13041035 | — |
反応手順
Cyanoacetic acid (1.75 g., 0.02 mole) was dissolved in 10 ml. of dioxane. In a five minute period 4-t-butylpiperidine (2.8 g., 0.02 mole) was added, the temperature rose to 25° C. from 15° C. obtained by prior cooling with an ice bath. The mixture which solidified became fluid upon the addition of 37% aqueous formaldehyde (3.6 g., 0.04 mole), the temperature rose to 30° C. and carbon dioxide evolution began. The mixture was stirred an additional 12 hours, was taken up in ether and the organic phase separated and washed with water. The dried ether solution was stripped of solvent to leave a solid residue product, 3.7 g. of practically analytical purity.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04254131 |
| 出典データセット | uspto-grants-1981_03 |
| ORD ID | ord-bcafefd463434a369923d6a6c2a36c1a |
| 出典メモ | uspto-grants-1981_03 |