反应详情

温度

160 °C

To a solution of (S)-ethyl 2-tert-butoxy-2-(7-(4-chlorophenyl)-2-(2-chloropyridin-4-yl)-5-methylbenzo[d]thiazol-6-yl)acetate (30 mg, 0.057 mmol) and 1H-indazole (6.0 mg, 0.052 mmol) in DMF (0.5 mL) was added K2CO3 (16.0 mg, 0.117 mmol) and 18-crown-6 (0.1 mg, 5.1×10−4 mmol). The reaction mixture was heated in a microwave at 160° C. for 1 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 60% ethyl acetate/hexanes) and then purified by reverse phase HPLC, eluting by 0-100% acetonitrile in H2O with 0.1% TFA to give the desired product. LCMS-ESI+ (m/z): [M+H]+ calcd for C34H32ClN4O3S: 611.2; found: 611.3.

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 60% ethyl acetate/hexanes)
7. custompurified by reverse phase HPLC
8. washeluting by 0-100% acetonitrile in H2O with 0.1% TFA