HRID2252031

反应详情

EQUATION

反应方程式

HRID 2252031 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 4,5-dibromo-2-methylimidazole (3.0 g, 12.5 mmol) in 25 mL DMF add sodium carbonate (2.0 g, 18.8 mmol) and benzyl bromide (1.64 mL, 13.8 mmol). Stir the solution at room temperature for 72 hours. Pour the reaction into water and extract with EtOAc. Wash the organic layer with water, saturated aqueous sodium chloride, and dry over sodium sulfate. Filter the mixture and concentrate to 3.8 g crude oil. Purify the oil by radial chromatography eluting with 40% EtOAc in hexanes. Concentrate the appropriate fractions to 3.1 g (75%) of the title compound as a colorless oil. MS(ES+): m/z=331.0 (M+H)+

WORKUP

后处理

  1. additionPour
  2. extractionextract with EtOAc
  3. washWash the organic layer with water, saturated aqueous sodium chloride
  4. dry with materialdry over sodium sulfate
  5. filtrationFilter the mixture
  6. concentrationconcentrate to 3.8 g crude oil
  7. customPurify the oil by radial chromatography
  8. washeluting with 40% EtOAc in hexanes
  9. concentrationConcentrate the appropriate fractions to 3.1 g (75%) of the title compound as a colorless oil