化工社化工社 化学情報印刷レポート · 研究参考用
Hydrochloric Acid → 3-acetyl-1-(4-iodo-2-methoxyphenyl)-5-methoxypyridazin-4(1H)-one
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | Tetrahydrofuran | HCID 8028 | — |
| 反応物 | 1-(4-iodo-2-methoxyphenyl)-N,5-dimethoxy-N-methyl-4-oxo-1,4-dihydropyridazine-3-carboxamide | HCID 59436205 | — |
| 生成物 | 3-acetyl-1-(4-iodo-2-methoxyphenyl)-5-methoxypyridazin-4(1H)-one | HCID 86686555 | — |
反応手順
To a solution of 1-(4-iodo-2-methoxyphenyl)-N,5-dimethoxy-N-methyl-4-oxo-1,4-dihydropyridazine-3-carboxamide (8.90 g) in THF (150 mL) was added dropwise 1M methylmagnesium bromide THF solution (30 mL) at −78° C., and the mixture was stirred for 20 min. To the reaction mixture was added 1M hydrochloric acid, and the mixture was extracted with ethyl acetate. The extract was washed with water and saturated brine, dried over anhydrous magnesium sulfate, and concentrated under reduced pressure. The residue was washed with ethyl acetate, and recrystallized from methanol/water to give the title compound (5.12 g).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US09090586B2 |
| 出典データセット | uspto-grants-2015_07 |
| ORD ID | ord-f72b8724a7504dfb83551c3d726fef6d |
| 出典メモ | uspto-grants-2015_07 |