反应详情

First, 2.42 g of 4-chlorobenzofuro[3,2-d]pyrimidine, 2.19 g of phenylboronic acid, 1.89 g of sodium carbonate, 0.10 g of bis(triphenylphosphine)palladium(II)dichloride (abbreviation: Pd(PPh3)2Cl2), 20 mL of water, and 20 mL of acetonitrile were put into a recovery flask equipped with a reflux pipe, and the air in the flask was replaced with argon. This reaction container was heated by 60-minute microwave irradiation (2.45 GHz, 100 W). After that, the obtained residue was suction-filtered with water and washed with hexane. The obtained solid was purified by flash column chromatography using a developing solvent in which the ratio of hexane to ethyl acetate was 2:1, so that Hpbfpm, which was the pyrimidine derivative to be produced, was obtained as a white powder in a yield of 45%. Note that the microwave irradiation was performed using a microwave synthesis system (Discover, manufactured by CEM Corporation). A synthesis scheme of Step 1 is illustrated in (d-1) below.

1. customequipped with a reflux pipe
2. temperatureThis reaction container was heated by 60-minute
3. custommicrowave irradiation (2.45 GHz, 100 W)
4. filtrationAfter that, the obtained residue was suction-filtered with water
5. washwashed with hexane
6. customThe obtained solid was purified by flash column chromatography
7. customto be produced
8. customwas obtained as a white powder in a yield of 45%
9. customNote that the microwave irradiation
10. customa microwave synthesis system (Discover, manufactured by CEM Corporation)
11. customA synthesis scheme of Step 1