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 | 1,4-Diazepan-6-ol | HCID 21114275 | — |
| 溶媒 | Ethanol | HCID 702 | — |
| 生成物 | 1-(6-Bromopyridin-2-yl)-1,4-diazepan-6-ol | HCID 86707088 | 54.4% |
反応手順
A mixture of 2-bromo-6-fluoropyridine (477 mg, 2.7 mmol), 1,4-diazepan-6-ol (350 mg, 3 mmol), and DIPEA (1.94 g, 15 mmol) in ethanol (10 mL) was heated at 100° C. for 16 hours. After it was cooled, the reaction mixture was concentrated under reduced pressure. The residue was diluted with EtOAc (100 mL) and washed with brine. The organic layer was dried over Na2SO4 and concentrated under reduced pressure to afford 1-(6-bromopyridin-2-yl)-1,4-diazepan-6-ol as a colorless oil (400 mg, 48.9%). MS (ESI) m/z: 272 [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-4a05fc6b800647e6bfba96bdba62fac7 |
|---|
| 出典メモ | uspto-grants-2016_09 |
|---|
