関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Hydrazine hydrate (1:1) | HCID 24654 | — |
| 反応物 | 3-(4-Cyclohexyloxy-phenyl)-2-hydroxy-4-oxo-octanoic acid ethyl ester | HCID 67375747 | — |
| 溶媒 | Acetic Acid | HCID 176 | — |
| 生成物 | 6-butyl-5-(4-cyclohexyloxy-phenyl)-2H-pyridazin-3-one | HCID 67375285 | — |
反応手順
To a stirred solution of the octanoic acid ethyl ester (105 mmol, 39.5 g) in glacial acetic acid (25.5 mL) was added hydrazine hydrate (525 mmol, 25.5 mL), and the reaction was heated at 100° C. for 12 h. After cooling, the volatiles were removed in vacuo, the residue was dissolved in ethyl acetate (300 mL). The organic layer was washed with water (100 mL), saturated NaHCO3 (3×100 mL), brine (100 mL), dried (Na2SO4), filtered, and concentrated under reduced pressure. The residue was recrystallized from a mixture of ethyl acetate (200 mL) and hexanes (300 mL) to afford 6-butyl-5-(4-cyclohexyloxy-phenyl)-2H-pyridazin-3-one.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US08431575B2 |
|---|
| 出典データセット | uspto-grants-2013_04 |
|---|
| ORD ID | ord-13fbcb4e18c04e66b853b2bcdb0dafdf |
|---|
| 出典メモ | uspto-grants-2013_04 |
|---|