関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Menthol | HCID 1254 | — |
| 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 ethyl (-)-menthyl ester | HCID 53871925 | 31.8% |
反応手順
To a mixture of 2-(pyrrol-1-yl)malonic acid diethyl ester (300.0 g) and (-)-menthol (417.0 g) was added tetraethyl titanate (10.0 g), and the resulting mixture was stirred at 110° C. for 19 hours. After removal of the (-)-menthol under reduced pressure, the residue was chromatographed on silica gel using n-hexane/ethyl acetate (50:1) as the eluent. Fractions containing the title compound were pooled and evaporated under reduced pressure to give the title compound (142.0 g, 31.8%) as a colorless oil.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US05258382 |
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| 出典データセット | uspto-grants-1993_11 |
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| ORD ID | ord-f14a8b62c6884870a484f598b5c82ebb |
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| 出典メモ | uspto-grants-1993_11 |
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