HRID432696

反应详情

EQUATION

反应方程式

HRID 432696 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

Under a nitrogen atmosphere, 2-(5-methyl-1H-tetrazol-1-yl)benzoic acid (89.7 g, 0.44 mol) was dissolved in acetone (1 L) and cesium carbonate (214.7 g, 0.66 mol) was added with vigorous stirring. Ethyl iodide (70.3 ml, 0.88 mol) was added dropwise and the reaction was heated to reflux for 4 hours. The reaction was cooled to room temperature and filtered. The acetone was removed in vacuo to yield a yellow solid which was dissolved in dichloromethane (800 ml) and washed with saturated sodium bicarbonate (200 ml). The organic fraction was dried (Na2SO4), filtered, and concentrated to yield 92.7 g of ethyl 2-(5-methyl-1H-tetrazol-1-yl)benzoate as a light yellow solid.

WORKUP

后处理

  1. temperaturethe reaction was heated
  2. temperatureto reflux for 4 hours
  3. filtrationfiltered
  4. customThe acetone was removed in vacuo
  5. customto yield a yellow solid which
  6. washwashed with saturated sodium bicarbonate (200 ml)
  7. dry with materialThe organic fraction was dried (Na2SO4)
  8. filtrationfiltered
  9. concentrationconcentrated