関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Diisopropylethylamine | HCID 81531 | — |
| 反応物 | 2-Bromo-6-fluoropyridine | HCID 639438 | — |
| 反応物 | Tert-butyl 1,4-diazepane-1-carboxylate | HCID 2756058 | — |
| 溶媒 | Ethanol | HCID 702 | — |
| 生成物 | tert-Butyl 4-(6-bromopyridin-2-yl)-1,4-diazepane-1-carboxylate | HCID 70700340 | 50.1% |
反応手順
A mixture of 2-bromo-6-fluoropyridine (500 mg, 2.8 mmol), tert-butyl 1,4-diazepane-1-carboxylate (568 mg, 2.8 mmol) in DIPEA (1.83 g, 14.2 mmol) in ethanol (10 mL) was heated at 100° C. for 16 hours. The reaction mixture was concentrated under reduced pressure and the residue was diluted with EtOAc (100 mL). The solution was washed with brine, dried over Na2SO4, and concentrated under reduced pressure to afford tert-butyl 4-(6-bromopyridin-2-yl)-1,4-diazepane-1-carboxylate as a colorless oil (500 mg, 50%). MS (ESI) m/z: 356 [M+H]+.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US09434725B2 |
|---|
| 出典データセット | uspto-grants-2016_09 |
|---|
| ORD ID | ord-3c81de5258514889bd3738db16a79614 |
|---|
| 出典メモ | uspto-grants-2016_09 |
|---|
