反应详情

温度

120 °C

Cs2CO3 (742 mg, 2.28 mmol) was added portionwise to a rt solution of 2-bromo-5-chloro-4-methyl-benzoic acid methyl ester (300 mg, 1.14 mmol) in DMF (3 mL) followed by 1H-1,2,3-triazole (0.1 mL, 1.71 mmol), Cu(I)I (13 mg, 0.068 mmol) and DMCDA (40 uL, 0.23 mmol). The resulting suspension was stirred at 120° C. for 4 h. The rxn mixture was quenched with 2M aq. HCl and extracted with EtOAc (3×). The combined org. layers were dried (Na2SO4), filtered and evaporated in vacuo to obtain the crude product that was purified by prep. HPLC (method C) to give the title compound A-1-15 as a pale yellow solid. LC-MS A: tR=0.72 min; [M(35Cl)+H]+=238.01.

1. customThe rxn mixture was quenched with 2M aq. HCl
2. extractionextracted with EtOAc (3×)
3. dry with materiallayers were dried (Na2SO4)
4. filtrationfiltered
5. customevaporated in vacuo
6. customto obtain the crude product that
7. customwas purified by prep