تفاعل #86175

معادلة التفاعل

2-bromo-6-fluoropyridine

1,4-diazepan-6-ol

DIPEA

→

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

المردود 54.4%

المذيبات

ethanol

ظروف التفاعل

المعالجة

1. 1
   درجة الحرارةAfter it was cooled
2. 2
   تركيزthe reaction mixture was concentrated under reduced pressure
3. 3
   workup.ADDITIONThe residue was diluted with EtOAc (100 mL)
4. 4
   غسيلwashed with brine
5. 5
   تجفيفThe organic layer was dried over Na2SO4
6. 6
   تركيزconcentrated under reduced pressure

الإجراء التجريبي

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]+.

المصدر