反应详情

A solution of 2.66 g of 1-(2-chlorobenzyl)-6-ethoxycarbonyl-2-methylbenzimidazole in 20 ml of tetrahydrofuran was slowly added to a solution of 1.54 g of lithium aluminum hydride in 20 ml of tetrahydrofuran at a temperature of from 20 to 25° C. Further, the mixture was stirred at room temperature for 1 hour. Thirty milliliters of tetrahydrofuran were added thereto to dilute the reaction solution. Lithium ammonium hydride was decomposed and solidified with a saturated aqueous solution of sodium sulfate, and the tetrahydrofuran layer was separated. The solvent was distilled off, and the residue was purified through silica-gel column chromatography (eluent: a mixture of chloroform and methanol at a ratio of 9:1) to give 1.45 g of 1-(2-chlorobenzyl)-6-hydroxymethyl-2-methylbenzimidazole.

1. additionto dilute the reaction solution
2. customthe tetrahydrofuran layer was separated
3. distillationThe solvent was distilled off
4. customthe residue was purified through silica-gel column chromatography (eluent
5. additiona mixture of chloroform and methanol at a ratio of 9:1)