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Ethane, 1-chloro-1-ethoxy- → 4,5-Dichloro-2-(3,4-dichlorophenyl)-1-(1-ethoxyethyl)pyrrole-3-carbonitril
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Ethane, 1-chloro-1-ethoxy- | HCID 23478 | — |
| 反応物 | 4,5-dichloro-2-(3,4-dichlorophenyl)-1H-pyrrole-3-carbonitrile | HCID 183555 | — |
| 反応物 | Potassium tert-butoxide | HCID 23665647 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | 4,5-Dichloro-2-(3,4-dichlorophenyl)-1-(1-ethoxyethyl)pyrrole-3-carbonitril | HCID 23359469 | 97.5% |
反応手順
To 4,5-dichloro-2-(3,4-dichlorophenyl)-pyrrole-3-carbonitrile (5.0 g, 0.016 mol) dissolved in 300 mL of tetrahydrofuran is added, portionwise, potassium t-butoxide (2.75 g, 0.025 mol) with ice cooling and stirring. The cooled mixture is treated with a solution of 1-chloroethyl ethyl ether (2.31 g, 0.021 mol) in 15 mL of tetrahydrofuran at 10° C. over a 5 minute period. The mixture is stirred for 1/2 hour at ambient temperatures, evaporated to a volume of 50 mL and poured into a mixture of 200 mL of ethyl acetate and 100 mL of water. The organic layer is separated, washed with water (2×100 mL), saturated NaCl solution (1×100 mL), dried over anhydrous magnesium sulfate and evaporated to give the title product 5.9 g, mp 124°-126° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05591765 |
| 出典データセット | uspto-grants-1997_01 |
| ORD ID | ord-112c0cca36bb4ebc9e2e1395a5fe5a64 |
| 出典メモ | uspto-grants-1997_01 |