反应详情

温度

90 °C

To a solution of compound (1H-benzo[d]imidazol-2-yl)(4-hydroxyphenyl)methanone (100 g, 0.42 mol) in anhydrous DMF (1.1 L) was added K2CO3 (145 g, 1.05 mol, 2.5 eq.) and 2,3-dichloropyrazine (75.08 g, 0.50 mol, 1.2 eq.). The reaction was stirred at 90° C. for 18 h. LCMS analysis of the reaction mixture showed that the reaction was complete. The reaction mixture was cooled to ambient temperature and ice-water (3 L) was added, stirred for 30 minutes. The resulting solid was filtered and washed with water (3 L) followed by MTBE (2×500 mL) and dried under vacuum. The solid was treated with 50% MTBE/DCM at 50° C. for 1 h and filtered hot, washed with 50% MTBE/DCM and dried under vacuum overnight to obtain product. Mother liquor was refluxed with 50% MTBE/DCM for 2 h and filtered hot and washed with 50% MTBE/DCM to get another batch of product. MS (ESI, pos. ion) m/z: 351.0 (M+1). IC50 (uM) +.

1. temperatureThe reaction mixture was cooled to ambient temperature
2. stirringstirred for 30 minutes
3. filtrationThe resulting solid was filtered
4. washwashed with water (3 L)
5. customdried under vacuum
6. additionThe solid was treated with 50% MTBE/DCM at 50° C. for 1 h
7. filtrationfiltered hot
8. washwashed with 50% MTBE/DCM
9. customdried under vacuum overnight
10. customto obtain product
11. filtrationfiltered hot
12. washwashed with 50% MTBE/DCM
13. customto get another batch of product