関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Nitric Acid | HCID 944 | — |
| 反応物 | Sulfuric Acid | HCID 1118 | — |
| 反応物 | 6-Amino-2,4-dimethyl-3-pyridinecarbonitrile | HCID 3793299 | — |
| 生成物 | 2-Amino4,6-dimethyl-3-nitro-5-pyridinecarbonitrile | HCID 54420031 | 55.2% |
反応手順
To 10 mL of H2SO4 (97%) kept in an ice-bath was added portionwise 2.45 g (16.6 mmol) of 2-amino-4,6-dimethyl-5-pyridinecarbonitrile (16) and it was stirred for 30 min. The resulting solution was heated at 55° C. and 1.2 mL (18.8 mmol) of HNO3 (d=1.41, 69-70%) was added dropwise. The solution was heated at 55°-60° C. for 3 h after addition of HNO3. It was cooled to room temperature and poured into 60 mL of ice-water. The yellow precipitate was filtered, washed with water, and dried to leave a yellow solid (1.76 g, 55%). 1H NMR (CDCl3), 2.612 (s, 3), 2.716 (s, 3), 6.51 (mb, 2).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US05863916 |
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| 出典データセット | uspto-grants-1999_01 |
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| ORD ID | ord-51ff5ba0bdc84da28ec8b40775622bd3 |
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| 出典メモ | uspto-grants-1999_01 |
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