化工社化工社 化学情報印刷レポート · 研究参考用
Bicyclo[3.2.1]octan-2-one → N-(Bicyclo[3.2.1]oct-2-yl)-N'-(4-methylpyridazino[4,5-b]indolizin-1-yl) 1,2-ethanediamine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Bicyclo[3.2.1]octan-2-one | HCID 107363 | — |
| 反応物 | HCID 20075511 | HCID 20075511 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 溶媒 | Dimethyl sulfoxide methanol | HCID 22036561 | — |
| 生成物 | N-(Bicyclo[3.2.1]oct-2-yl)-N'-(4-methylpyridazino[4,5-b]indolizin-1-yl) 1,2-ethanediamine | HCID 20075513 | — |
反応手順
Following the procedure of Example 12, bicyclo[3.2.1]octan-2-one in methanol (3 to 4 mL) was added to a solution of N-(4-methylpyridazino[4,5-b]indolizin-1-yl)-1,2-ethanediamine hydrochloride in methanol/DMSO (90 mL:30 mL) which had been heated to boiling and then allowed to cool. After stirring at room temperature overnight, the title compound was obtained as the free base after column chromatography (silica gel, 4:1 methylene chloride:methanol to 100% methanol containing ammonium hydroxide) and recrystallized from isopropyl ether. The compound was converted to the dihydrochloride salt by ethanolic HCl, mp 339°-344° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04985560 |
| 出典データセット | uspto-grants-1991_01 |
| ORD ID | ord-af0ce9f90e2948de88d97fd7b1f2795a |
| 出典メモ | uspto-grants-1991_01 |