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Triethylamine → 1-Methyl-beta-oxo-alpha-(2,6-dichlorophenylcarbamoyl)-2-pyrrolpropionitrile
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | 1,3-Dichloro-2-isocyanatobenzene | HCID 604537 | — |
| 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-(2,6-dichlorophenylcarbamoyl)-2-pyrrolpropionitrile | HCID 20285425 | — |
反応手順
To the filtered solution of 4.4 g of 2,6-dichlorophenylisocyanate in 30 ml of toluene is added 2.5 g of 1-methyl-β-oxo-2-pyrrolpropionitrile and 2.1 g of triethylamine while stirring. The mixture is allowed to stand overnight at room temperature, whereupon it is filtered. The solids are washed with toluene and diethyl ether, taken up in 50 ml of methanol and the solution poured into the mixture of 6 ml of 5 N hydrochloric acid and 300 ml of water. The crystals formed are collected, washed with water, dried, triturated with ethanol, and recrystallized from methanol, to yield the 1-methyl-β-oxo-α-(2,6-dichlorophenylcarbamoyl)-2-pyrrolpropionitrile melting at 196°-199°.
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-aa5d06143fbb44aea1ef74dd2804a70f |
| 出典メモ | uspto-grants-1981_03 |