反应详情

27 mg of 6-(2-cyclopropylpyrimidin-4-yl)-2-(2-trimethylsilanylethoxymethyl)-4-[1-(2-trimethylsilanylethoxymethyl)-1H-benzimidazol-2-yl]-2H-pyridazin-3-one are dissolved in 2.5 ml of 4M hydrochloric acid solution in dioxane and 1 ml of ethanol and stirred at room temperature for 2 days. The solvent is then distilled off, and the residue is dissolved in 2 ml of dichloromethane and 1 ml of trifluoroacetic acid and again stirred at room temperature for 3 h. Distillation off is then repeated, and the residue is dissolved in 1 ml of 2M sodium hydroxide solution and 2 ml of water, and the mixture is stirred at room temperature for 10 h. For workup, it is neutralized with 2M hydrochloric acid, the volatile components are distilled off, and the crude product is purified by RP HPLC (acetonitrile (+0.05% HCOOH)/water (+0.05% HCOOH)).

1. distillationThe solvent is then distilled off
2. dissolutionthe residue is dissolved in 2 ml of dichloromethane
3. distillationDistillation
4. dissolutionthe residue is dissolved in 1 ml of 2M sodium hydroxide solution
5. stirring2 ml of water, and the mixture is stirred at room temperature for 10 h
6. distillationthe volatile components are distilled off
7. customthe crude product is purified by RP HPLC (acetonitrile (+0.05% HCOOH)/water (+0.05% HCOOH))