反应详情

温度

60 °C

To a solution of 1.45 g of 4-(4,4,5,5-tetramethyl-[1,3,2]dioxaborolan-2-yl)-phenylamine, 1.86 mL of triethylamine and 162 mg of 4-dimethlaminopyridine in 150 mL of tetrahydrofuran at 20° C. is added 1 g of 1-fluoro-2-isocyanato-4-methylbenzene. The reaction is stirred for 3 hours 30 minutes at 60° C., and then concentrated to dryness under reduced pressure. The residue is taken up in a mixture of water and dichloromethane. The organic phase is washed with 1N HCl solution and then dried over magnesium sulfate and concentrated to dryness under reduced pressure. 2.13 g of a white powder of 1-(2-fluoro-5-methylphenyl)-3-[4-(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl)phenyl]urea are obtained, the characteristics of which are as follows:

1. concentrationconcentrated to dryness under reduced pressure
2. additionThe residue is taken up in a mixture of water and dichloromethane
3. washThe organic phase is washed with 1N HCl solution
4. dry with materialdried over magnesium sulfate
5. concentrationconcentrated to dryness under reduced pressure