反应详情

To a solution of 5-bromo-2-fluoro-benzoic acid (500 mg, 2.28 mmol) in CH2Cl2 (15 mL) at 0° C. are added methyl 3-amino-2,4-dimethylbenzoate (409 mg, 2.28 mmol, see preparation 10) and N,N-diisopropylethylamine (737.6 mg, 5.71 mmol). After stirring the reaction mixture for 10 minutes, 1-propanephosphonic acid cyclic anhydride (50% solution in ethyl acetate, 1.74 g, 2.74 mmol) is added via syringe and stirred at 50° C. After 16 hours, the solvent is removed under reduced pressure and the residue is triturated with MeOH to give the title compound as a white solid (450 mg, 51.8%). Mass spectrum (m/z): 380.2 (M+1).

1. stirringstirred at 50° C
2. waitAfter 16 hours
3. customthe solvent is removed under reduced pressure
4. customthe residue is triturated with MeOH