反应详情

温度

80 °C

Add 3 mg (0.01 mmol) trans-bis(dicyclohexylamine)palladium(II) acetate [T. Bin, J. Org. Chem. 2004, 69, 4330-4335] to a mixture of 100 mg (0.22 mmol) 6-{[6-bromo-5-(4-methoxyphenyl)furo[2,3-d]pyrimidin-4-yl]amino}hexanoic acid methyl ester, 47 mg (0.34 mmol) 3-fluorophenylboronic acid and 145 mg (0.45 mmol) caesium carbonate in 5 ml dioxan, and stir for 16 h at 80° C. After adding 95 mg (0.45 mmol) potassium phosphate, a further 47 mg (0.34 mmol) 3-fluorophenylboronic acid and a spatula tip of trans-bis(dicyclohexylamin)palladium(II) acetate, stir the reaction mixture for a further 4 h at 80° C. Then filter the reaction mixture and purify directly by preparative RP-HPLC (gradient: water/acetonitrile). 57 mg (53% of theor.) of the desired product is obtained.

1. filtrationThen filter the reaction mixture
2. custompurify directly by preparative RP-HPLC (gradient: water/acetonitrile)