関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Methyl 1-methylpyrrol-2-acetate | HCID 103992 | — |
| 反応物 | Oxo-P-tolyl-acetonitrile | HCID 641326 | — |
| 生成物 | Methyl 1-methyl-5-(4-methylbenzoyl)-1H-pyrrole-2-acetate | HCID 118468 | 398.8% |
反応手順
A mixture of 5.0 g (0.034 mole) of 4-methylbenzoylcyanide and 0.8 g (0.005 mole) of methyl 1-methyl-pyrrole-2-acetate was added over 4 hours from a heated addition funnel to a sample of 3.8 g (0.025 mole) of methyl 1-methylpyrrole-2-acetate at 180° through which nitrogen was bubbled. The mixture was heated for six more hours after the addition was complete. The reaction was cooled and dissolved in methylene chloride-toluene. The organic solution was washed with 10 percent sodium hydroxide solution and saturated brine and dried (MgSO4). The solvent was evaporated in vacuo and the residue recrystallized twice from methanol to give 5.41 g (69 percent yield) of white crystalline methyl 1-methyl-5-(4-methyl-benzoyl)-pyrrole-2-acetate, mp 118°-120° C. The solid state IR spectrum was identical to authentic material.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US04255335 |
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| 出典データセット | uspto-grants-1981_03 |
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| ORD ID | ord-6485920042fe41719bbc666e5ea2aa49 |
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| 出典メモ | uspto-grants-1981_03 |
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