反应详情

A mixture of 1-(4-Amino-10-aza-tricyclo[6.3.1.02.7]dodeca-2,4,6-trien-10-yl)-2,2,2-trifluoro-ethanone (158 g, 0.624 mmol) (see International Publication Nos. WO01/076576A2, WO01/062736A1, WO99/35131 and European Patent No. EP 1078637), 1,4-dioxane (1.00 mL), N-{3-[(2-Chloro-5-trifluoromethyl-pyrimidin-4-ylamino)-methyl]-pyridin-2-yl}-N-methyl-methanesulfonamide (247 mg, 0.624 mmol) and DIAE (255 mL, 1.47 mmol) was heated to 110° C. under a gentle flow of nitrogen. After sixteen hours, the mixture was concentrated, and the resulting residue was purified over silica (95:5:0.5 CHCl3:CH3OH:NH4OH) to provide (+/−) N-Methyl-N-(3-{[2-(10-trifluoroacetyl-10-aza-tricyclo[6.3.1.02.7]dodeca-2(7),3,5-trien-4-ylamino)-5-trifluoromethyl-pyrimidin-4-ylamino]-methyl}-pyridin-2-yl)-methanesulfonamide (3) as a white foam (78 mg, 0.124 mmol, 20%). C26H25F6N7O3S LC/MS (Method F) 630.3 (MH+); 19F NMR (D6-DMSO) δ −60.38, −67.99 (1:1 ratio) ppm.

1. waitAfter sixteen hours
2. concentrationthe mixture was concentrated
3. customthe resulting residue was purified over silica (95:5:0.5 CHCl3:CH3OH:NH4OH)