反应详情

温度

90 °C

In a 10 mL reaction vial, 5-(6-chloro-3-methylpyridin-2-yl)-1-methyl-1H-indazole (100 mg, 0.389 mmol) was dissolved in dioxane (5 mL) at rt. The solution was bubbled with argon for 5 min. Then Sn2(n-Bu)6 (0.253 mL, 0.508 mmol), LiCl (100 mg, 2.38 mmol), Pd(PPh3)2Cl2 (27 mg, 0.039 mmol) and Pd(PPh3)4 (45 mg, 0.039 mmol) were added sequentially. The resulting reaction mixture was sealed and heated to 90° C. in oil bath. To this mixture, a solution of (S)-ethyl 2-(2-bromo-7-(4-chlorophenyl)-5-methylbenzo[d]thiazol-6-yl)-2-tert-butoxyacetate (289 mg, 0.583 mmol) in dioxane (5 mL) was added slowly through syringe pump over 1.5 h. The resulting reaction mixture was stirred at 100° C. in oil bath for 16 h. The reaction was then diluted with EtOAc (20 mL) and filtered to remove solid. The filtrate was concentrated and purified on silica gel column with 0-20% EtOAc/Hex to afford product as. LCMS-ESI+: calc'd for: C36H35ClN4O3S: 639.2, 640.2, 641.2 (M+H+); found: 639.1, 640.1, 641.1 (M+H+).

1. customIn a 10 mL reaction vial
2. customThe solution was bubbled with argon for 5 min
3. customThe resulting reaction mixture
4. customwas sealed
5. customThe resulting reaction mixture
6. filtrationfiltered
7. customto remove solid
8. concentrationThe filtrate was concentrated
9. custompurified on silica gel column with 0-20% EtOAc/Hex
10. customto afford product as