반응 #86175

반응 방정식

2-bromo-6-fluoropyridine

1,4-diazepan-6-ol

DIPEA

→

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

수율 54.4%

용매

ethanol

반응 조건

후처리

1. 1
   온도After it was cooled
2. 2
   농축the reaction mixture was concentrated under reduced pressure
3. 3
   workup.ADDITIONThe residue was diluted with EtOAc (100 mL)
4. 4
   세척washed with brine
5. 5
   건조The organic layer was dried over Na2SO4
6. 6
   농축concentrated under reduced pressure

실험 절차

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]+.

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