関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Phosphorus oxychloride | HCID 24813 | — |
| 反応物 | Phosphorus pentachloride | HCID 24819 | — |
| 反応物 | Sodium Bicarbonate | HCID 516892 | — |
| 反応物 | 2-Hydroxy-5-nitro-3-(trifluoromethyl)pyridine | HCID 2775095 | — |
| 生成物 | 2-Chloro-5-nitro-3-(trifluoromethyl)pyridine | HCID 3849140 | — |
反応手順
A mixture of 5-nitro-3-(trifluoromethyl)pyridin-2(1H)-one 3 (1.50 g, 7.21 mmol), POCl3 (2.76 g, 18.02 mmol) and PCl5 (1.4 g, 10.09 mmol) is heated to about 110-120° C. for 8 hours and then poured into ice water. The mixture is neutralized with solid NaHCO3 and extracted with ethyl acetate (3×40 ml). The combined organic phases is dried over Na2SO4 and all solvents removed under reduced pressure to obtain 2-chloro-5-nitro-3-(trifluoromethyl)pyridine 4.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US09388159B2 |
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| 出典データセット | uspto-grants-2016_07 |
|---|
| ORD ID | ord-546b2a4cb24049ce8707c4ee63f1b7a6 |
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| 出典メモ | uspto-grants-2016_07 |
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