関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Benzyl Alcohol | HCID 244 | — |
| 反応物 | diethyl 2-(1H-pyrrol-1-yl)malonate | HCID 2782128 | — |
| 触媒 | Titanium(IV)ethoxide | HCID 2724286 | — |
| 生成物 | 2-(Pyrrol-1-yl)malonic acid dibenzyl ester | HCID 54532374 | 87.3% |
反応手順
To a solution of 2-(pyrrol-1-yl)malonic acid diethyl ester (75.7 g) in benzyl alcohol (200 ml) was added tetraethyl titanate (3.0 g), and the resulting mixture was stirred at 110° C. for 15 hours. After removal of the benzyl alcohol under reduced pressure, the residue was chromatographed on silica gel using n-hexane/ethyl acetate (10:1) as the eluent. Fractions containing the title compound were pooled and evaporated under reduced pressure. The residue was recrystallized from ethyl acetate/n-hexane to give the title compound (102.5 g, 87.3%) as colorless crystals, mp 48.5°-49° 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-32045007fac441dfb7bc1bce30e13674 |
|---|
| 出典メモ | uspto-grants-1993_11 |
|---|