反应详情

温度

110 °C

To a solution of (S)-ethyl 2-(2-bromo-7-(4-chlorophenyl)-5-methylbenzo[d]thiazol-6-yl)-2-tert-butoxyacetate (36.7 mg, 0.076 mmol) and 2,7-naphthyridin-1(2H)-one (14.0 mg, 0.092 mmol) in DMF (0.9 mL) was added CuI (9.0 mg, 0.046 mmol) and trans-N1,N2-dimethylcyclohexane-1,2-diamine (15 μL, 0.092 mmol) and K2CO3 (21.0 mg, 0.152 mmol). The reaction was heated at 110° C. for 2 h. After cooling, the reaction mixture was diluted with EtOAc, extracted with H2O, brine, dried over Na2SO4, filtered and concentrated and purified by flash column chromatography (silica gel, 0 to 100% ethyl acetate/hexanes) to give the desired product. LCMS-ESI+ (m/z): [M+H]+ calcd for C30H29ClN3O4S: 562.2; found: 562.3.

1. temperatureAfter cooling
2. extractionextracted with H2O, brine
3. dry with materialdried over Na2SO4
4. filtrationfiltered
5. concentrationconcentrated
6. custompurified by flash column chromatography (silica gel, 0 to 100% ethyl acetate/hexanes)