化工社化工社 化学情報印刷レポート · 研究参考用
Triethylamine → 2-[5-Bromo-4-(1,1,3,3-tetramethylbutylamino)-6-oxopyridazin-1(6H)-yl]-N-(pyridin-4-ylmethyl)acetamide
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | 2,5,5-Trimethylhexan-2-amine | HCID 17776513 | — |
| 反応物 | 1,4-Dioxane--water (1/1) | HCID 21886435 | — |
| 反応物 | 2-(4,5-Dibromo-6-oxopyridazin-1(6H)-yl)-N-(pyridin-4-ylmethyl)acetamide | HCID 59574387 | — |
| 生成物 | 2-[5-Bromo-4-(1,1,3,3-tetramethylbutylamino)-6-oxopyridazin-1(6H)-yl]-N-(pyridin-4-ylmethyl)acetamide | HCID 59574376 | 25% |
反応手順
2-(4,5-Dibromo-6-oxopyridazin-1(6H)-yl)-N-(pyridin-4-ylmethyl)acetamide (50 mg, 124 μmol) in dioxane-water (1:1, 2 mL) was stirred with triethylamine (52 μL, 372 μmol) and 2,5,5-trimethylhexan-2-amine (16 mg, 112 μmol) at 90° C. for 26 hours. After completion of the reaction, the solvent was removed by vacuum distillation, and the residue was mixed with saturated aqueous sodium chloride and extracted with chloroform three times. The combined organic layer was dried over anhydrous magnesium sulfate, and the solvent was removed by vacuum distillation. The resulting residue was purified by silica gel chromatography (chloroform/methanol=10/1) to give the desired product (13 mg, 25% yield).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08440666B2 |
| 出典データセット | uspto-grants-2013_05 |
| ORD ID | ord-6e9ef58306234159a76720ed54d5fd8b |
| 出典メモ | uspto-grants-2013_05 |