化工社化工社 化学情報印刷レポート · 研究参考用
Chloroacetone → 6-Chloro-2-methyl-7-phenyl-imidazo[1,2-b]pyridazine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Chloroacetone | HCID 6571 | — |
| 反応物 | 6-Chloro-5-phenylpyridazin-3-amine | HCID 56953654 | — |
| 反応物 | 6-Chloro-4-phenylpyridazin-3-amine | HCID 76848713 | — |
| 溶媒 | Water | HCID 962 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | 6-Chloro-2-methyl-7-phenyl-imidazo[1,2-b]pyridazine | HCID 86692116 | — |
反応手順
The mixture of 6-chloro-5-phenyl-pyridazin-3-yl-amine and 6-Chloro-4-phenyl-pyridazin-3-yl-amine (intermediate example Int-1-0, step 3, 65 g=316 mmol) in 65 mL tetrahydrofurane and 650 mL water was heated with 74.5 g (800 mmol) chloroacetone in analogy to the synthesis of the intermediate example Int-1-0, step 4, for 18 hours at reflux. After the usual work up and purification of the residue by chromatography (Biotage Isolera, Kronlab 8 cm, eluents: dichloromethane/methanol) and subsequent crystallization (methyl-tert.butylether/hexane) 11.69 g (30.4%) of the title compound were obtained.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08987273B2 |
| 出典データセット | uspto-grants-2015_03 |
| ORD ID | ord-f31d3977efed4a85b61908caad28f507 |
| 出典メモ | uspto-grants-2015_03 |