HRID70795
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
CONDITIONS
反应条件
- 温度
- 140 °C
PROCEDURE
实验过程
A mixture of 4,5,6,7-tetrahydro-1H-benzimidazol-2-yl acetonitrile (8.5 g), methyl 2-oxocyclopentanecarboxylate (7.5 g) and ammonium acetate (20.3 g) was stirred at 140° C. for 2 hours. The reaction mixture was cooled to room temperature, water was added, and extraction was performed with chloroform. The organic layer was washed with a saturated brine, dried over anhydrous sodium sulfate, and concentrated reduced pressure. The residue was solidified using hexane/EtOAc to obtain 11-hydroxy-2,3,6,7,8,9-hexahydro-1H-cyclopenta[4,5]pyrido[1,2-a]benzimidazole-4-carbonitrile (2.56 g).
WORKUP
后处理
- temperatureThe reaction mixture was cooled to room temperature
- extractionextraction
- washThe organic layer was washed with a saturated brine
- dry with materialdried over anhydrous sodium sulfate
- concentrationconcentrated reduced pressure