関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | Calcium Carbonate | HCID 10112 | — |
| 反応物 | Methyl isocyanide | HCID 11646 | — |
| 反応物 | 2-Methylbenzoyl chloride | HCID 70276 | — |
| 溶媒 | Acetone | HCID 180 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | N-methyl-2-(2-methylphenyl)-2-oxoacetamide | HCID 15239356 | 96.6% |
反応手順
A mixture of 2-methylbenzoyl chloride (1.55 g) and methyl isocyanide (492 mg) was stirred at 60° C. for 6 hours. Then, the mixture was diluted with acetone (20 ml), and water (4 ml) and calcium carbonate (1.00 g) were added. The stirring of the resulting mixture was continued for 1 hour. The mixture was neutralized with dilute hydrochloric acid and extracted with methylene chloride. The organic layer was washed with saturated brine and dried over anhydrous magnesium sulfate. The solvent was evaporated under reduced pressure. The residue was subjected to column chromatography on silica gel and eluted with hexane-ethyl acetate (5:1) to obtain the title compound (1.71 g, Yield: 96.6%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US05414122 |
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| 出典データセット | uspto-grants-1995_05 |
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| ORD ID | ord-336b3b8c2eb143d68f7aa0398be0a69a |
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| 出典メモ | uspto-grants-1995_05 |
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