HRID1698605
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 mixture of 7-(1-ethylprop-1-en-1-yl)-1-methyl-4-(trifluoromethyl)-1,3-dihydro-2H-benzimidazol-2-one (486 mg, 1.71 mmol), 10% palladium on carbon (200 mg) and acetic acid (5 ml) was hydrogenated under 5 atom of hydrogen at 50° C. for 2 h. Catalyst was filtered off and filtrates were concentrated in vacuo. Aqueous saturated sodium bicarbonate was added to the residue and extracted with ethyl acetate. The extracts were washed with water, dried over magnesium sulfate and concentrated in vacuo. The residue was purified by recrystallization from diisopropylether/n-hexane to give 350 mg (1.22 mmol, 72%) of the title compound as a white powder.
WORKUP
后处理
- filtrationCatalyst was filtered off
- concentrationfiltrates were concentrated in vacuo
- additionAqueous saturated sodium bicarbonate was added to the residue
- extractionextracted with ethyl acetate
- washThe extracts were washed with water
- dry with materialdried over magnesium sulfate
- concentrationconcentrated in vacuo
- customThe residue was purified by recrystallization from diisopropylether/n-hexane