HRID1698582
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
A solution of 3-{4-chloro-2-[(4-chloro-2-methoxy-6-methylphenyl)amino]-1-methyl-1H-benzimidazol-7-yl}-2,4-dimethylpentan-3-ol (75 mg, 0.17 mmol) in trifluoroacetic acid (3 mL) was heated at 70° C. for 1 h. After cooling, the reaction mixture was concentrated in vacuo, neutralized with saturated sodium hydrogen carbonate, and extracted with ethyl acetate. The organic layer was dried over magnesium sulfate, filtered, and concentrated in vacuo. The residue was purified by preparative HPLC eluting with a 5-95% acetonitrile/water gradient mixture to give the title compound (58 mg, 80%).
WORKUP
后处理
- temperatureAfter cooling
- concentrationthe reaction mixture was concentrated in vacuo
- extractionextracted with ethyl acetate
- dry with materialThe organic layer was dried over magnesium sulfate
- filtrationfiltered
- concentrationconcentrated in vacuo
- customThe residue was purified by preparative HPLC
- washeluting with a 5-95% acetonitrile/water gradient mixture