反应详情

A n-pentane solution of tert-butyl lithium (1.46 M, 0.5 ml) was added to a solution of methyl 4-chloro-2-[(4-chloro-2-methoxy-6-methylphenyl)amino]-1-methyl-1H-benzimidazole-7-carboxylate (100 mg, 0.23 mmol) in diethyl ether (5 ml) at −78° C. and stirred for 1 h. The reaction mixture was diluted with water (5 mL), stirred at room temperature for 0.5 h and extracted with ethyl acetate. The organics was dried over magnesium sulfate, filtered, and concentrated in vacuo. The residue was purified by preparative HPLC. The resultant was neutralized with aqueous sodium hydrogen carbonate and extracted with ethyl acetate. The organics were dried over magnesium sulfate, filtered, and concentrated in vacuo to give 5 mg (0.010 mmol, 5%) of the title compound.

1. stirringstirred at room temperature for 0.5 h
2. extractionextracted with ethyl acetate
3. dry with materialThe organics was dried over magnesium sulfate
4. filtrationfiltered
5. concentrationconcentrated in vacuo
6. customThe residue was purified by preparative HPLC
7. extractionextracted with ethyl acetate
8. dry with materialThe organics were dried over magnesium sulfate
9. filtrationfiltered
10. concentrationconcentrated in vacuo