反应详情

温度

50 °C

The reaction solution of ethyl 4-methylthiazole-2-carboxylate of preparation 83 (240 mg, 1.40 mmol), NBS (277 mg, 1.14 mmol) in CH3CN (5 mL) was heated at 50° C. for overnight under nitrogen. ˜20% starting material was present by LCMS. Additional portion of NBS (70 mg) was added. The reaction solution was heated at 60° C. for 4 hr, diluted with EtOAc (30 ml), washed with water (2×20 mL), brine, dried over sodium sulfate and purified with a silica gel column by ISCO CombiFlash® chromatography eluting with 0%-20% EtOAc/Heptane to give the title compound as a yellowish oil (177 mg, 50.5%).

1. temperatureThe reaction solution was heated at 60° C. for 4 hr
2. washwashed with water (2×20 mL), brine
3. dry with materialdried over sodium sulfate
4. custompurified with a silica gel column by ISCO CombiFlash® chromatography
5. washeluting with 0%-20% EtOAc/Heptane