反应详情

温度

160 °C

In an 8 mL vial equipped with a stir bar was placed 5-(3′-chloro-2-fluoro-6-methoxy-biphenyl-3-ylmethyl)-2-fluoro-pyridine (P-456,150 mg, 0.434 mmol), azetidine (88.0 uL, 1.30 mmol) and 1,8-diazabicyclo[5.4.0]undec-7-ene (306 uL, 2.17 mmol). The mixture was heated to 160° C. for 1 hour and then cooled to room temperature. The reaction mixture was treated with water (4 mL) and 1M HCl (6 mL). The aqueous portion was extracted with dichloromethane (2×30 mL), the organic portions were combined, washed with brine (15 mL), dried (MgSO4) and concentrated to produce 156 mg of P-569 as a white solid in 94% yield.

1. customIn an 8 mL vial equipped with a stir bar
2. temperaturecooled to room temperature
3. extractionThe aqueous portion was extracted with dichloromethane (2×30 mL)
4. washwashed with brine (15 mL)
5. dry with materialdried (MgSO4)
6. concentrationconcentrated