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2-Chloro-3-nitropyridine → 2-Isothiocyanato-3-nitropyridine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 2-Chloro-3-nitropyridine | HCID 79613 | — |
| 反応物 | Isothiocyanatopotassium | HCID 10931372 | — |
| 溶媒 | Acetic Acid | HCID 176 | — |
| 生成物 | 2-Isothiocyanato-3-nitropyridine | HCID 19043345 | — |
反応手順
A 10 g sample of 2-chloro-3-nitropyridine, an 8 g sample of potassium isothiocyanate, and 75 ml of acetic acid were combined and refluxed for 2 h. The reaction mixture was then cooled and poured into 400 ml of ice/H2O. The resulting solid was washed with water, redissolved in ethyl acetate and washed (4×) with water. The ethyl acetate solution was then treated with activated carbon, dried over anhydrous Na2SO4, filtered and evaporated to dryness to provide 3.72 g of the title compound. m.p.=115°-118° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05362722 |
| 出典データセット | uspto-grants-1994_11 |
| ORD ID | ord-4b772b145bc242f9a799c02bc4429d65 |
| 出典メモ | uspto-grants-1994_11 |