HRID1747311
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
To a solution of 1-(4-Methyl-benzo[b]thiophen-3-ylmethyl)-1,3-dihydro-benzimidazol-2-one (0.1 g, 0.34 mmol) in AcCN (2 mL) and DMF (1 mL) were added ethyl propiolate (0.04 mL, 0.34 mmol) and DMAP (0.02 mL, 0.17 mmol). The reaction mixture was stirred at room temperature for 2 h. When the reaction was complete, the reaction mixture was diluted with CH2Cl2 and washed with water. The organic phase was dried over Na2SO4 and concentrated. The resulting residue was purified by silica gel prep TLC using 95:5 CH2Cl2:MeOH as an eluent to afford 0.11 g of the desired product as a white solid. LCMS (ESMS): m/z 393.13 (M+H+).
WORKUP
后处理
- washwashed with water
- dry with materialThe organic phase was dried over Na2SO4
- concentrationconcentrated
- customThe resulting residue was purified by silica gel prep TLC