関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | 1,3-Dichloro-5,5-dimethylhydantoin | HCID 8360 | — |
| 反応物 | Sodium Hydroxide | HCID 14798 | — |
| 反応物 | Tert-butyl 4-(6-bromopyridin-3-yl)-1,4-diazepane-1-carboxylate | HCID 22478562 | — |
| 反応物 | HCID 178418306 | HCID 178418306 | — |
| 溶媒 | Pentane | HCID 8003 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | 1-(6-Chloro-3-pyridyl)-4-tert-butoxycarbonyl homopiperazine | HCID 22478487 | — |
反応手順
A stirred solution of 1-(6-Bromo-3-pyridyl)-4-tert-butoxycarbonyl homopiperazine (3.6 g, 10 mmol) in tetrahydrofuran (200 ml) was cooled to −78° C. Tert-butyllithium (14.7 ml, 1.5 M) in pentane was added during 10 min, followed by stirring for 5 min at −78° C. 1,3-Dichloro-5,5-dimethylhydantoin (1.97 g, 10 mmol) was added in small portions. The mixture was stirred for 0.5 min. Aqueous sodium hydroxide was added (100 ml, 4 M), and the reaction was allowed reach room temperature. The mixture was extracted twice with diethyl ether (100 ml) Chromatography on silica gel with a mixture of petroleum:ethyl acetate (1:1) gave the title compound as free base. Yield 1.7 g, 55%.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US06825189B1 |
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| 出典データセット | uspto-grants-2004_11 |
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| ORD ID | ord-d75e475319114f4989e4078b8186e13a |
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| 出典メモ | uspto-grants-2004_11 |
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