HRID505783
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 (0.15 M) of methyl 6-cyclohexyl-5-phenyl-4H-thieno[3,2-b]pyrrole-2-carboxylate in DMF at 0° C. was treated with NaH (3.5 eq., 60% dispersion in mineral oil), and the suspension was stirred at RT for 30 min then it was treated with benzyl bromide (2.5 eq.). The reaction mixture was stirred at RT for 3 h then it was diluted with Et2O and water then the layers were separated and the aqueous phase was extracted with AcOEt. The combined organic phase was dried and concentrated giving a residue that was purified by flash chromatography on silica gel (1:10 MeOH/DCM) affording the title compound (22%) as a solid.
WORKUP
后处理
- stirringThe reaction mixture was stirred at RT for 3 h
- customthe layers were separated
- extractionthe aqueous phase was extracted with AcOEt
- customThe combined organic phase was dried
- concentrationconcentrated
- customgiving a residue that
- customwas purified by flash chromatography on silica gel (1:10 MeOH/DCM)