HRID1249814

反应详情

EQUATION

反应方程式

HRID 1249814 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
-10 °C

PROCEDURE

实验过程

4-Cyanobenzylbromide (1.05 g, 5.39 mmol) was added to a solution of 4-bromo-2-methylimidazole-5-carboxaldehyde (1.02 g, 5.39 mmol) (Step A) in dimethylacetamide (15 mL). The solution was cooled to −10° C. and powdered potassium carbonate (0.745 g, 5.39 mmol) added. The reaction was stirred at −10° C. for 2 h, and a further 4 h at 20° C. The reaction was diluted with water and extracted with ethyl acetate. The organic phase was washed with water, saturated brine, and dried over magnesium sulfate. Solvent evaporation yielded a white solid. 1H NMR (CDCl3, 400 MHz) 8 9.68 (1H, s), 7.64 (2H, d, J=7 Hz), 7.15 (2H, d, J=7Hz), 5.59 (2H, s), 2.40 (3H, s).

WORKUP

后处理

  1. customa further 4 h
  2. customat 20° C
  3. extractionextracted with ethyl acetate
  4. washThe organic phase was washed with water, saturated brine
  5. dry with materialdried over magnesium sulfate
  6. customSolvent evaporation
  7. customyielded a white solid