関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | N-bromobutanimide | HCID 67184 | — |
| 反応物 | 1-(Pyridin-3-yl)-4-tert-butoxycarbonylhomopiperazine | HCID 10802494 | — |
| 溶媒 | Acetonitrile | HCID 6342 | — |
| 生成物 | Tert-butyl 4-(6-bromopyridin-3-yl)-1,4-diazepane-1-carboxylate | HCID 22478562 | — |
反応手順
1-(3-Pyridyl)-4-tert-butoxycarbonyl homopiperazine (25.0 g, 90.1 mmol) was solved in acetonitrile (400 ml) and cooled to 0° C. N-Bromosuccinimide (19.3 g, 108.2 mmol) was added during 10 min. Water (400 ml) was added and the mixture was extracted twice with diethyl ether (200 ml). Chromatography on silica gel with a mixture of petroleum: ethyl acetate (1:1) gave the title compound as free base. Yield 18.7 g, 58%.
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-ef958457bc004d1daadb6440c6752247 |
|---|
| 出典メモ | uspto-grants-2005_05 |
|---|
