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Acetic Anhydride → Ethyl 1-phenyl-3-pyrrolecarboxylate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Acetic Anhydride | HCID 7918 | — |
| 反応物 | Ethyl propiolate | HCID 12182 | — |
| 反応物 | (Formylanilino)acetic acid | HCID 7099130 | — |
| 溶媒 | Hexane | HCID 8058 | — |
| 生成物 | Ethyl 1-phenyl-3-pyrrolecarboxylate | HCID 22738020 | — |
反応手順
A mixture of 2.69 g (15 mmole) of N-formyl-N-phenyl-glycine prepared in Reference Example 3, 5.47 g (55.8 mmole) of ethyl propiolate, and 15 ml of acetic anhydride was stirred using a magnetic stirrer over an oil bath at 130° C. for 22 hours. The reaction mixture was concentrated under vacuum. 22 ml of toluene was added to the residue and the mixture was evaporated under reduced pressure. This procedure was repeated to obtain a brown oily substance. This oily substance was purified using silica gel column chromatography (No. 9385 silica gel, manufactured by Merck Co., eluted with ethyl acetate:hexane=1:5 v/v) to obtain 2.8949 (yield 89.6%) of a light-yellow oil of the title compound.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05684161 |
| 出典データセット | uspto-grants-1997_11 |
| ORD ID | ord-79c22996605c4231a1a6f9a9954cc030 |
| 出典メモ | uspto-grants-1997_11 |