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1,2-Dimethoxyethane → 1-[6-(N-Pyrrolidinyl)-3-pyridyl]-4-tert-butoxycarbonyl homopiperazine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 1,2-Dimethoxyethane | HCID 8071 | — |
| 反応物 | Pyrrolidine | HCID 31268 | — |
| 反応物 | Tert-butyl 4-(6-bromopyridin-3-yl)-1,4-diazepane-1-carboxylate | HCID 22478562 | — |
| 反応物 | Potassium tert-butoxide | HCID 23665647 | — |
| 触媒 | HCID 178418397 | HCID 178418397 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | 1-[6-(N-Pyrrolidinyl)-3-pyridyl]-4-tert-butoxycarbonyl homopiperazine | HCID 22478457 | — |
反応手順
A stirred solution of 1-(6-Bromo-3-pyridyl)-4-tert-butoxycarbonyl homopiperazine (0.71 g, 2.0 mmol), pyrrolidine (2.0 g, 20 mmol), potassium tert-butoxide (0.45 g, 4.0 mmol), tetrakis(triphenylphosphine)palladium(0) (0.12 g, 0.10 mmol) and 1.2-dimethoxyethane was stirred at reflux overnight. Water (40 ml) was added and the mixture was extracted twice with ethyl acetate (20 ml) Chromatography on silica gel with a mixture of petroleum: ethyl acetate (1:1) gave the title compound as free base. Yield 0.21 g, 30%.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06897219B2 |
| 出典データセット | uspto-grants-2005_05 |
| ORD ID | ord-dbbda2a566ed48e284b0973d208317b6 |
| 出典メモ | uspto-grants-2005_05 |