Реакция #86175

Уравнение реакции

2-bromo-6-fluoropyridine

1,4-diazepan-6-ol

DIPEA

→

1-(6-bromopyridin-2-yl)-1,4-diazepan-6-ol

Выход 54.4%

Растворители

ethanol

Условия реакции

Обработка

1. 1
   ТемператураAfter it was cooled
2. 2
   Концентрированиеthe reaction mixture was concentrated under reduced pressure
3. 3
   workup.ADDITIONThe residue was diluted with EtOAc (100 mL)
4. 4
   Промывкаwashed with brine
5. 5
   СушкаThe organic layer was dried over Na2SO4
6. 6
   Концентрированиеconcentrated under reduced pressure

Методика

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]+.

Источник