HRID571158

反应详情

EQUATION

反应方程式

HRID 571158 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A 100 mL reactor was charged with the aqueous solution of triethylammonium 1,1,2,2-tetrafluoro-4-(2-methyl-acryloyloxy)-butane-1-sulfonate obtained by the 3rd step, and a solution of 20.2 g (0.056 mole) of triphenylsulfonium bromide and 100 g of chloroform, followed by 3 hours of stirring at room temperature. Subsequently, an organic layer was separated, and the thus obtained organic layer was rinsed with 100 g of water four times. Subsequently, it was rinsed with 100 g of diisopropyl ether three times thereby precipitating a solid. Upon performing filteration, the solid was dried, thereby obtaining 32.5 g of a target triphenylsulfonium 1,1,2,2-tetrafluoro-4-(2-methyl-acryloyloxy)-butane-1-sulfonate. It exhibited a purity of 93% at this time (most of a balance of 7% was the solvent, i.e., diisopropyl ether), and a yield of 97% taken over from the 3rd step.

WORKUP

后处理

  1. customobtained by the 3rd step
  2. customSubsequently, an organic layer was separated
  3. washthe thus obtained organic layer was rinsed with 100 g of water four times
  4. washSubsequently, it was rinsed with 100 g of diisopropyl ether three times
  5. customthereby precipitating a solid
  6. customthe solid was dried