反应详情

A solution of 2-methylbenzylzinc chloride (1.95 ml, 973 μmol, 0.5 M in THF) was added dropwise at −78° C. to a solution of B-OM-9-BBN (0.97 ml, 973 μmol, 1 M in hexane). The cooling bath was removed and the mixture was stirred at room temperature for 30 min. DMF (2 ml) was added, followed by the compound of step 5 (50 mg, 97.3 μmol), palladium(II) acetate (2.18 mg, 9.73 μmol) and S-PHOS (7.99 mg, 19.5 μmol). The reaction mixture was heated to 100° C. and stirred for 4 h. The mixture was diluted with water and extracted with EA. The organic layer was separated, dried over sodium sulfate, filtered and evaporated under reduced pressure. The residue was purified by preparative HPLC. The eluate was lyophilized overnight to give 14 mg of the title compound.

1. customThe cooling bath was removed
2. additionDMF (2 ml) was added
3. temperatureThe reaction mixture was heated to 100° C.
4. stirringstirred for 4 h
5. extractionextracted with EA
6. customThe organic layer was separated
7. dry with materialdried over sodium sulfate
8. filtrationfiltered
9. customevaporated under reduced pressure
10. customThe residue was purified by preparative HPLC
11. waitThe eluate was lyophilized overnight