化工社化工社 化学情報印刷レポート · 研究参考用
Ethylenediamine → Brimonidine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Ethylenediamine | HCID 3301 | — |
| 反応物 | 5-Bromo-6-isothiocyanatoquinoxaline | HCID 4460274 | — |
| 溶媒 | Benzene | HCID 241 | — |
| 生成物 | Brimonidine | HCID 2435 | — |
反応手順
The 5-bromo-6-isothiocyanato-quinoxaline (3.5 g.) is directly dissolved in benzene (400 ml) and added dropwise to a well-stirred solution of ethylene diamine (15 g.) in benzene (50 ml). During a period of about two hours, an oil separates as a lower layer. The upper benzene layer is poured off and the oil is washed with diethyl ether and then dissolved in methanol (500 ml). The methanolic solution is refluxed until hydrogen sulfide evolution ceases. The methanolic solution is concentrated in vacuo to a volume of approximately 100 ml upon which a yellow solid precipitates. The precipitate is collected by filtration and recrystallized from methanol to afford of (5-Bromo-quinoxalin-6-yl)-(4,5-dihydro-1H-imidazol-2-yl)-amine: m.p. 250-251 C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08859551B2 |
| 出典データセット | uspto-grants-2014_10 |
| ORD ID | ord-7a4d27cd378f47d6b1bdf1e189cb3221 |
| 出典メモ | uspto-grants-2014_10 |