反应详情

温度

100 °C

To a solution of [(2R,5R)-5-(5-amino-2-fluoro-phenyl)-2,5-dimethyl-2-trifluoromethyl-5,6-dihydro-2H-[1,4]oxazin-3-yl]-carbamic acid tert-butyl ester (CAS registry 1262859-70-0) (138 mg, 0.34 mmol) and 4,7-dichloro-pyrido[3,2-d]pyrimidine (CAS registry 917757-12-1) (75 mg, 0.374 mmol) in tBuOH (2 ml) was added 0.1 ml 4N HCl in dioxane and the reaction mixture was heated in a microwave oven for 1 h at 100° C. The reaction mixture was basified with saturated NaHCO3 solution and the product was extracted with EtOAc. Combined extracts were washed with brine, dried over MgSO4, filtered and concentrated. The crude product was dissolved in THF, acidified with 1N HCl in Et2O, and concentrated. The remaining yellow solid was two times triturated with Et2O and subsequently dried to afford the title compound as light yellow amorphous solid.

1. extractionthe product was extracted with EtOAc
2. washCombined extracts were washed with brine
3. dry with materialdried over MgSO4
4. filtrationfiltered
5. concentrationconcentrated
6. dissolutionThe crude product was dissolved in THF
7. concentrationconcentrated
8. customtriturated with Et2O
9. customsubsequently dried