関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | Benzene, 1-isocyanato-4-nitro- | HCID 66012 | — |
| 反応物 | 3-(1-Methyl-1H-pyrrol-2-yl)-3-oxopropanenitrile | HCID 2777170 | — |
| 溶媒 | Dimethyl Sulfoxide | HCID 679 | — |
| 溶媒 | Toluene | HCID 1140 | — |
| 生成物 | 1-Methyl-beta-oxo-alpha-(p-nitrophenylcarbamoyl)-2-pyrrolpropionitrile | HCID 20285405 | — |
反応手順
The solution of 4.9 g of the 1-methyl-β-oxo-2-pyrrolpropionitrile in 50 ml of toluene, 5 ml of dimethylsulfoxide and 4 g of triethylamine is treated with the solution of 5.7 g of p-nitrophenylisocyanate in the minimum amount of toluene while stirring. After standing overnight it is evaporated and the residue taken up in methanol. The solution is filtered, diluted with water and 6 ml of triethylamine, washed with ethyl acetate, and the washings extracted once with 5% aqueous sodium hydroxide. The combined aqueous solutions are acidified with 5 N hydrochloric acid and the precipitate collected. It is washed with water, triturated with methanol-ethanol and recrystallized from dimethylformamide, to yield the 1-methyl-β-oxo-α-(p-nitrophenylcarbamoyl)-2-pyrrolpropionitrile melting at 245°-250° with decomposition.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US04256759 |
|---|
| 出典データセット | uspto-grants-1981_03 |
|---|
| ORD ID | ord-4724d9ac5eb64a77a9945cca3c2ce5fa |
|---|
| 出典メモ | uspto-grants-1981_03 |
|---|