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Trichloroacetyl chloride → 2-(2-Trichloroacetylpyrrol-1-yl)malonic acid diethyl ester
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Trichloroacetyl chloride | HCID 6420 | — |
| 反応物 | diethyl 2-(1H-pyrrol-1-yl)malonate | HCID 2782128 | — |
| 溶媒 | Chloroform | HCID 6212 | — |
| 生成物 | 2-(2-Trichloroacetylpyrrol-1-yl)malonic acid diethyl ester | HCID 10547163 | 89% |
反応手順
To a solution of 2-(pyrrol-1-yl)malonic acid diethyl ester (100.0 g) in chloroform (100 ml) was added trichloroacetyl chloride (161.4 g), and the resulting mixture was refluxed for 15 hours. The reaction mixture was concentrated under reduced pressure, and the residue was dissolved in ethyl acetate. The solution was washed with 10% aqueous sodium carbonate solution and then with saturated aqueous sodium chloride solution, dried over anhydrous sodium sulfate, and evaporated under reduced pressure. The residue was recrystallized from isopropyl ether to give the title compound (146.4 g, 89.0%) as colorless crystals, mp 67°-69° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05258382 |
| 出典データセット | uspto-grants-1993_11 |
| ORD ID | ord-fb9e6de47aa948b9b0384c1ba25e19a7 |
| 出典メモ | uspto-grants-1993_11 |