反应详情

温度

70 °C

NBS (747 mg, 4.20 mmol) was added in portions to a 50 mL sealed tube reactor containing methyl 4-(1-methyl-1H-pyrazol-5-yl)-2-thiophenecarboxylate (860 mg, 3.48 mmol) [prepared according to the procedure of Example 37] in Tetrahydrofuran (THF) (17 mL) at room temperature. The mixture was heated to 70° C. for 1.5 hours, cooled to room temperature and partitioned between CHCl3 and H2O. The organic layer was dried with Na2SO4, adsorbed onto silica and purified via column chromatography (20-40% EtOAc/hexanes) affording the title compound (867 mg, 83%): LC-MS (ES) m/z=303 (M+H)+.

1. customsealed tube reactor
2. customprepared
3. customat room temperature
4. temperaturecooled to room temperature
5. custompartitioned between CHCl3 and H2O
6. dry with materialThe organic layer was dried with Na2SO4
7. custompurified via column chromatography (20-40% EtOAc/hexanes)