HRID875202
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
产物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
To a solution of N-methylimidazole (10.0 g, 122 mmol) in acetonitrile (120 mL) was added benzoyl chloride (14.1 mL, 122 mmol) followed by triethylamine (17.0 mL, 122 mmol), while keeping the internal temperature at 5° C. The mixture was stirred 18 h at room temperature. After filtration, the filtrate was concentrated in vacuo, diluted with ethyl acetate (200 mL) and sequentially washed with sat. aq. sodium bicarbonate (150 mL), water (100 mL) and brine (100 mL). The organic layer was dried over MgSO4 and concentrated in vacuo.to afford (1-methyl-1H-imidazol-2-yl)(phenyl)methanone [21.0 g, yield 83%; HPLC/MS: m/z=187 (M+H); log P(HCOOH)=1.38].
WORKUP
后处理
- customat 5° C
- filtrationAfter filtration
- concentrationthe filtrate was concentrated in vacuo
- additiondiluted with ethyl acetate (200 mL)
- washsequentially washed with sat. aq. sodium bicarbonate (150 mL), water (100 mL) and brine (100 mL)
- dry with materialThe organic layer was dried over MgSO4
- concentrationconcentrated in vacuo.to