反应详情

A mixture of 8.84 g of N-(5-amino-4-chloro-2-fluorophenyl)-3,4,5,6-tetrahydrophthalimide, 12.6 g of 4-acetoxytetrahydrofuran-3-yl 2-bromopropionate, 3.02 g of sodium hydrogencarbonate and 3 ml of xylene was heated under stirring at 150° to 160° C. for 4 hours. Adding ethyl acetate to the reaction mixture while it remained warm, the resulting mixture was washed with water, subsequently with aqueous saturated sodium chloride solution, and dried over anhydrous magnesium sulfate. After distilling off the solvent, the residue was purified by chromatography on a silica gel column (development solvent: ethyl acetate/hexane=1/2), to obtain 4.88 g of a compound described in Table 1 (No. 10) (33 %).

1. temperaturewas heated
2. washthe resulting mixture was washed with water, subsequently with aqueous saturated sodium chloride solution
3. dry with materialdried over anhydrous magnesium sulfate
4. distillationAfter distilling off the solvent
5. customthe residue was purified by chromatography on a silica gel column (development solvent: ethyl acetate/hexane=1/2)