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Water → Butyl 1,6-dihydro-6-oxo-3-pyridazinecarboxylate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | Sulfuric Acid | HCID 1118 | — |
| 反応物 | 6-Hydroxypyridazine-3-carboxylic Acid | HCID 305970 | — |
| 溶媒 | 1-Butanol | HCID 263 | — |
| 溶媒 | Butyl Acetate | HCID 31272 | — |
| 生成物 | Butyl 1,6-dihydro-6-oxo-3-pyridazinecarboxylate | HCID 12346430 | 170.5% |
反応手順
A solution of 6-oxo-1,6-dihydropyridazine-3-carboxylic acid (British patent no. 856409) (52 g, 0.33 mol) in nBuOAc (80 ml) and butanol (80 ml) was treated with concentrated sulphuric acid (5 ml). The mixture was heated at reflux under a Dean-Stark trap. After 5 hours water production had ceased. The reaction was allowed to cool to ambient temperature and after standing overnight, the precipitate was filtered, washed with diethyl ether and dried to give butyl 6-oxo-1,6-dihydropyridazine-3-carboxylate as a white solid (55.2 g, 85%) m.p. 81-83° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06365603B1 |
| 出典データセット | uspto-grants-2002_04 |
| ORD ID | ord-94d09b112ac748a396e5418bcc6a2711 |
| 出典メモ | uspto-grants-2002_04 |