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p-Toluenesulfonic acid → Methyl 3-amino-4-methyl-5-(1H-pyrrol-1-yl)benzoate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | p-Toluenesulfonic acid | HCID 6101 | — |
| 反応物 | 2,2-Diethoxytetrahydrofuran | HCID 358290 | — |
| 反応物 | Sodium Acetate | HCID 517045 | — |
| 反応物 | Methyl 3,5-diamino-4-methylbenzoate | HCID 18984069 | — |
| 溶媒 | Acetic Acid | HCID 176 | — |
| 溶媒 | Ethanol | HCID 702 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | Methyl 3-amino-4-methyl-5-(1H-pyrrol-1-yl)benzoate | HCID 20290401 | — |
反応手順
A mixture of 18 g. of methyl 3,5-diamino-4-methylbenzoate, 0.7 g. of p-toluenesulfonic acid, 8.2 g. of sodium acetate, 32 g. of diethoxytetrahydrofuran, 10 ml of glacial acetic acid, 100 ml. of ethanol and 100 ml. of water was boiled at reflux for 3 hours. The alcohol was removed in vacuo and the residue extracted with ethyl acetate. The ethyl acetate solution was washed with water, dried over sodium sulfate and evaporated. By purification of the residue over aluminum oxide with ethyl acetate and recrystallization from high-boiling petroleum ether, there was obtained methyl 3-amino-4-methyl-5-(pyrrol-1-yl)benzoate, having a melting point of 112° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04039543 |
| 出典データセット | uspto-grants-1977_08 |
| ORD ID | ord-f416015af10e465481b4c8c9412673ac |
| 出典メモ | uspto-grants-1977_08 |