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Triethylamine → 2-[3-(5-Bromo-3-methylpyrid-2-yl)propylamino]-3-nitro-5-(pyrid-3-ylmethyl)pyridine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | 2-(3-Aminopropyl)-5-bromo-3-methylpyridine | HCID 19851781 | — |
| 反応物 | 2-Chloro-3-nitro-5-(pyrid-3-ylmethyl)pyridine hydrochloride | HCID 19851787 | — |
| 触媒 | 2-(3-Aminopropyl)-5-bromo-3-methylpyridine | HCID 19851781 | — |
| 溶媒 | Ethanol | HCID 702 | — |
| 生成物 | 2-[3-(5-Bromo-3-methylpyrid-2-yl)propylamino]-3-nitro-5-(pyrid-3-ylmethyl)pyridine | HCID 19851791 | 197.5% |
反応手順
2-(3-Aminopropyl)-5-bromo-3-methylpyridine (5 g), 2-chloro-3-nitro-5-(pyrid-3-ylmethyl)pyridine hydrochloride (4.45 g) and triethylamine (10 ml) were refluxed together in ethanol (200 ml) for 5.5 hr. A further addition of 2-(3-aminopropyl)-5-bromo-3-methylpyridine (0.5 g) was made and refluxing was continued for a further 2.5 hr. The reaction mixture was then concentrated to dryness giving a yellow oil (13.59 g). The oil was chromatographed on silica in first methanol/chloroform 1:19 increasing the polarity to 1:9. The product was recrystallised from chloroform/petroleum ether (40°-60° C.) to give the title compound (5.11 g), m.p. 105°-106° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04863933 |
| 出典データセット | uspto-grants-1989_09 |
| ORD ID | ord-caf7841f161a412c91b18e0d52fd35c8 |
| 出典メモ | uspto-grants-1989_09 |