HRID875202

反应详情

EQUATION

反应方程式

HRID 875202 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

  1. customat 5° C
  2. filtrationAfter filtration
  3. concentrationthe filtrate was concentrated in vacuo
  4. additiondiluted with ethyl acetate (200 mL)
  5. washsequentially washed with sat. aq. sodium bicarbonate (150 mL), water (100 mL) and brine (100 mL)
  6. dry with materialThe organic layer was dried over MgSO4
  7. concentrationconcentrated in vacuo.to