反应详情

130 μl (2.2 mMol) methyl isocyanate are added to a solution of 300 mg (0.68 mMol) 6-(2-amino-pyrimidin-4-yloxy)-naphthalene-1-carboxylic acid (4-fluoro-3-trifluoromethyl-phenyl)-amide (Step 10.3) in 10 ml THF in a sealed vessel. The mixture is stirred at 100° C. for 11 days (another 1.1 eq. of Me-NCO is added on day 8 and 9). Then the reaction mixture is diluted with EtOAc and water, the aq. phase separated off and extracted twice with EtOAc. The organic layers are washed with water and brine, dried (Na2SO4) and partially concentrated. Precipitation with hexane, filtration and re-crystallization from boiling THF/CH3CN gives the title compound: m.p.: 233-234° C.

1. additionis added on day 8 and 9)
2. customthe aq. phase separated off
3. extractionextracted twice with EtOAc
4. washThe organic layers are washed with water and brine
5. dry with materialdried (Na2SO4)
6. concentrationpartially concentrated
7. customPrecipitation
8. filtrationwith hexane, filtration and re-crystallization