反应详情

温度

60 °C

To a solution of (S)-ethyl 2-(2-(2-(1H-indazol-5-yl)pyridin-4-yl)-7-(4-chlorophenyl)-5-methylbenzo[d]thiazol-6-yl)-2-tert-butoxyacetate (20 mg, 0.0327 mmol) in DMF (1 mL) was added Cs2CO3 (53 mg, 0.163 mmol), methyl 2-chloro-2,2-difluoroacetate (4 μL, 0.039 mmol). The reaction mixture was heated at 60° C. overnight. Then more methyl 2-chloro-2,2-difluoroacetate (6 μL, 0.058 mmol) was added and heated at 60° C. for 1 day. The reaction mixture was washed by water, extracted by EtOAc, the organic phase was dried over MgSO4, filtered, concentrated down, purified by silica gel column, eluting by 0-50% EtOAc in hexanes to give (S)-ethyl 2-tert-butoxy-2-(7-(4-chlorophenyl)-2-(2-(1-(difluoromethyl)-1H-indazol-5-yl)pyridin-4-yl)-5-methylbenzo[d]thiazol-6-yl)acetate LCMS-ESI+: calc'd for C35H31ClF2N4O3S: 661.2 (M+H+); found: 661.2; and (S)-ethyl 2-tert-butoxy-2-(7-(4-chlorophenyl)-2-(2-(2-(difluoromethyl)-2H-indazol-5-yl)pyridin-4-yl)-5-methylbenzo[d]thiazol-6-yl)acetate. LCMS-ESI+: calc'd for C35H31ClF2N4O3S: 661.2 (M+H+); found: 661.3.

1. temperatureheated at 60° C. for 1 day
2. washThe reaction mixture was washed by water
3. extractionextracted by EtOAc
4. dry with materialthe organic phase was dried over MgSO4
5. filtrationfiltered
6. concentrationconcentrated down
7. custompurified by silica gel column
8. washeluting by 0-50% EtOAc in hexanes