HRID80472

反应详情

EQUATION

反应方程式

HRID 80472 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

8.53 g of 2,2-difluoroethanol are added to a solution of 17.31 g of methyl 5-fluoro-2-nitrobenzoate, 9.64 g of NEt3 and 32.71 g of 2,8,9-triisobutyl-2,5,8,9-tetraaza-1-phosphabicyclo[3.3.3]undecane in 250 ml of anhydrous THF. The mixture is stirred at AT for 30 min. The solvent is evaporated under reduced pressure. Water is added and extraction is carried out with AcOEt. The extract is washed with a 1N aqueous HCl solution, with water and then with a saturated NaCl solution. It is dried over MgSO4 and filtered, and the solvent is evaporated under reduced pressure to give 21 g of the expected product.

WORKUP

后处理

  1. customThe solvent is evaporated under reduced pressure
  2. additionWater is added
  3. extractionextraction
  4. washThe extract is washed with a 1N aqueous HCl solution, with water
  5. dry with materialIt is dried over MgSO4
  6. filtrationfiltered
  7. customthe solvent is evaporated under reduced pressure