関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | 2-Nitrophenylacetonitrile | HCID 11888 | — |
| 反応物 | Sodium hydride | HCID 24758 | — |
| 反応物 | 4,6-Dimethoxy-2-(methylsulfonyl)pyrimidine | HCID 838363 | — |
| 溶媒 | Water | HCID 962 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | 2-(4,6-Dimethoxypyrimidine-2-yl)-2-(2-nitrophenyl)acetonitrile | HCID 18417990 | 79.2% |
反応手順
50 g (0.31 M) of 2-(2-nitrophenyl)acetonitrile was dissolved in 500 ml of dimethylformamide. Thereto was added 24.7 g (0.62 M) of 60% sodium hydride. The mixture was stirred at room temperature for 2 hours. Then, 68 g (0.31 M) of 4,6-dimethoxy-2-methanesulfonylpyrimidine was added. The mixture was stirred at 80° C. for 1 hour to give rise to a reaction. The reaction mixture was poured into water, followed by neutralization with dilute hydrochloric acid. The mixture was subjected to extraction with ethyl acetate. The extract was washed with water, dried and subjected to vacuum distillation to remove the solvent. The residue was recrystallized from ethanol to obtain 73.3 g (yield: 79%) of 2-(4,6-dimethoxypyrimidine-2-yl)-2-(2-nitrophenyl)acetonitrile as a white powder (melting point: 88 to 89° C.).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US06458748B1 |
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| 出典データセット | uspto-grants-2002_10 |
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| ORD ID | ord-dd022a877f0f4698bbe28d430fdf74a2 |
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| 出典メモ | uspto-grants-2002_10 |
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