反应详情

A mixture of 4-[3-(1H-benzoimidazol-2-yl)-phenyl]-piperazine-1-carboxylic acid tert-butyl ester (0.83 g, 2.20 mmol) (obtained as described in method B) and NaH 60% oil (0.11 g, 4.39 mmol) in THF (10 mL) was stirred at room temperature for 1 h. Methyl iodide (0.27 mL, 4.39 mmol) was added and the resulting solution was stirred overnight. Water (15 mL) was added to the reaction solution, then the suspension was neutralized with 1N HCl and extracted with EtOAc (3×40 mL) The combined organic layers were dried (Na2SO4), filtered, and concentrated under reduced pressure. The residue was triturated with Et2O and the solid obtained filtered, to give 0.76 g (88%) of the title compound.

1. stirringthe resulting solution was stirred overnight
2. extractionextracted with EtOAc (3×40 mL) The combined organic layers
3. dry with materialwere dried (Na2SO4)
4. filtrationfiltered
5. concentrationconcentrated under reduced pressure
6. customThe residue was triturated with Et2O
7. customthe solid obtained
8. filtrationfiltered