反应详情

温度

60 °C

To a mixture of 1.00 g (3.86 mmol) of 2,4-dichloro-6,7-dimethoxyquinazoline, 1.14 g (4.63 mmol) of 3-(N-t-butoxycarbonylamino)phenyl borate, tetrahydrofuran (25 mL), and 2 M sodium carbonate aqueous solution (5 mL) were added palladium acetate (8.84 mg) and 1,1′-bis(diphenylphosphino)ferrocene (21.4 mg) in this order, and the mixture was stirred at 60° C. for 6.5 hours under a nitrogen atmosphere. The reaction solution was allowed to cool, and ethyl acetate (25 mL) and 5% w/w sodium chloride solution (20 mL) were added to extract the organic layer. The organic layer was washed twice with 5% w/w sodium chloride solution (20 mL) and then concentrated under reduced pressure. To the concentration residue were added ethyl acetate (1 mL) and 2-propanol (4 mL), and the mixture was suspended by stirring at 40° C. for 0.5 hours. The suspension was cooled, and the precipitated crystals were collected by filtration and dried to give 1.48 g of a target product (yield: 91.5%, HPLC purity: 99.02%).

1. temperatureto cool
2. extractionto extract the organic layer
3. washThe organic layer was washed twice with 5% w/w sodium chloride solution (20 mL)
4. concentrationconcentrated under reduced pressure
5. additionTo the concentration residue were added ethyl acetate (1 mL) and 2-propanol (4 mL)
6. stirringby stirring at 40° C. for 0.5 hours
7. temperatureThe suspension was cooled
8. filtrationthe precipitated crystals were collected by filtration
9. customdried