反应详情

To a solution of 2-amino-5-cyanobenzotrifluoride (1.0 g, 5.37 mmol, 1 eq) and benzyl bromide (2.55 mL, 21.5 mmol, 4.0 eq) in dry DMF (10 mL) was added at rt NaH (970 mg, 21.5 mmol, 4 eq) portion-wise under Ar(g). The reaction mixture was stirred at rt overnight, and was then partitioned with H2O (30 mL) and extracted with EtOAc (5×20 mL) and CH2Cl2 (20 mL). The combined organic extracts were dried over MgSO4 and the solvent was removed in vacuo. The residue was further purified by silica gel column chromatography with hexane/EtOAc (1:0-9:1) to yield the product, 2, as a pale yellow solid (1.66 g, 85%).

1. customwas then partitioned with H2O (30 mL)
2. extractionextracted with EtOAc (5×20 mL) and CH2Cl2 (20 mL)
3. dry with materialThe combined organic extracts were dried over MgSO4
4. customthe solvent was removed in vacuo
5. customThe residue was further purified by silica gel column chromatography with hexane/EtOAc (1:0-9:1)
6. customto yield the product, 2