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Hydrogen Peroxide → 2-Carboxy-6-chloropyridine 1-oxide
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Hydrogen Peroxide | HCID 784 | — |
| 反応物 | 6-Chloropicolinic acid | HCID 20812 | — |
| 溶媒 | Trifluoroacetic acid | HCID 6422 | — |
| 生成物 | 2-Carboxy-6-chloropyridine 1-oxide | HCID 53681338 | 67% |
反応手順
To a solution of 6-chloro-2-pyridinecarboxylic acid (14.8 g, 0.093 mol, for preparation, see Delarge, II. Farmaco-Ed.Sc., 1967, 22, 1069) in trifluoroacetic acid (110 ml) was added 75 ml of 30% aqueous hydrogen peroxide solution. The mixture was heated to 60° for 2 hours, cooled to room temperature and poured onto ice water. The white precipitate was filtered and was washed well with water to yield 10.8 g (67%) of the title compound of this preparation. mp 168°-170° C. 1H NMR (CDCl3): δ 7.46 (1H, d, J=8), 7.77 (1H, dd, J=8, 8), 8.01 (1H, d, J=8).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05789408 |
| 出典データセット | uspto-grants-1998_08 |
| ORD ID | ord-19fb74ca5ccc480c85a1d82d3c14c559 |
| 出典メモ | uspto-grants-1998_08 |