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Triethylamine → 1-Methyl-beta-oxo-alpha-(p-methoxyphenylcarbamoyl)-2-pyrrolpropionitrile
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | 1-Isocyanato-4-methoxybenzene | HCID 79443 | — |
| 反応物 | 3-(1-Methyl-1H-pyrrol-2-yl)-3-oxopropanenitrile | HCID 2777170 | — |
| 溶媒 | Toluene | HCID 1140 | — |
| 生成物 | 1-Methyl-beta-oxo-alpha-(p-methoxyphenylcarbamoyl)-2-pyrrolpropionitrile | HCID 14555704 | — |
反応手順
The suspension of 2.0 g of the 1-methyl-β-oxo-2-pyrrolpropionitrile in 50 ml of toluene and 1.6 g of triethylamine is treated with 2.1 g of p-methoxyphenylisocyanate. The mixture is warmed gently until all is dissolved and allowed to stand overnight at room temperature. It is evaporated, the residue is taken up in methanol and combined with 10 ml of 10% aqueous sodium hydroxide and 250 ml of water. The alkaline solution is filtered, acidified with 5 N hydrochloric acid and the precipitate formed collected. It is washed with water, dried, triturated with warm methanol-ethyl acetate, and recrystallized from ethyl acetate, to yield the 1-methyl-β-oxo-α-(p-methoxyphenylcarbamoyl)-2-pyrrolpropionitrile melting at 192°-193°.
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-bd67a2403f5947ea99ebdfd823a2528c |
| 出典メモ | uspto-grants-1981_03 |