HRID991594

反应详情

EQUATION

反应方程式

HRID 991594 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

4-amino-2-methylbenzimidazole (0.4 g, 2.7 mmol) and 2-ethyl-6-methylbenzylchloride (0.46 g, 2.7 mmol) were dissolved in 10 ml dimethoxyethane. Sodium carbonate (0.5 g, 4.7 mmol) and (0.2 g, 4.7 mmol) of potassium iodide were added to the solution. The reaction mixture was refluxed to for 2 h. Inorganic salts were removed by filtration and washed with dimethoxyethane. The filtrate was evaporated to dryness. The residue was purified by column chromatography on silica gel. The product was eluted with a 50:50 mixture of methylene chloride and ethyl acetate. There was obtained 0.21 g of the title compound. (1H-NMR, 400 MHz, CDCl3): 1.1 (t, 3H), 2.35 (s, 3H), 2.45 (s, 3H), 2.70 (q, 2H), 4.35 (s, 2H), 4.45 (bs, 1H), 6.55 (d, 1H), 6.75 (d, 1H), 6.95-7.20 (m, 4H).

WORKUP

后处理

  1. temperatureThe reaction mixture was refluxed to for 2 h
  2. customInorganic salts were removed by filtration
  3. washwashed with dimethoxyethane
  4. customThe filtrate was evaporated to dryness
  5. customThe residue was purified by column chromatography on silica gel
  6. washThe product was eluted with a 50:50 mixture of methylene chloride and ethyl acetate