反应详情

温度

100 °C

A 100-mL round-bottomed flask equipped with a reflux condenser was charged with 206f (108 mg, 0.30 mmol), 3-(acetoxymethyl)-2-(1-oxo-3,4,6,7,8,9-hexahydropyrazino[1,2-a]indol-2(1H)-yl)pyridin-4-ylboronic acid 113i (115 mg, 0.30 mmol), Pd(dppf)Cl2 (15 mg, 0.015 mmol), K3PO4 (135 mg, 0.60 mmol), sodium acetate trihydrate (90 mg, 0.60 mmol) in acetonitrile (10 mL) and water (0.5 mL). The system was evacuated and refilled with N2. The reaction mixture was heated at 100° C. for 2 h. It was then cooled to room temperature and filtered. The filtrate was concentrated under reduced pressure and the resulting residue was purified by silica-gel column chromatography eluting with 25:1 dichloromethane/methanol to afford 206g (90 mg, 52%) as a yellow brown solid. MS-ESI: [M+H]+ 624.2.

1. customA 100-mL round-bottomed flask equipped with a reflux condenser
2. customThe system was evacuated
3. additionrefilled with N2
4. temperatureIt was then cooled to room temperature
5. filtrationfiltered
6. concentrationThe filtrate was concentrated under reduced pressure
7. customthe resulting residue was purified by silica-gel column chromatography
8. washeluting with 25:1 dichloromethane/methanol