HRID2061305

反应详情

EQUATION

反应方程式

HRID 2061305 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

About 8 g of the diphenyl-4-hydroxyphenylsulfonium trifluoromethanesulfonate salt manufactured in the synthesis example 3 and about 9.05 g of a cyclohexanecarboxylic acid-2,2-difluoro-2-sulfo-ethyl ester sodium salt were dissolved in about 100 ml of an MC and about 100 ml of water, and a synthesis reaction (see Equation 12 below) was performed while strongly stirring for about three hours. In this instance, a process of the synthesis reaction was observed by 19F NMR using a small amount of an extracted organic phase. The organic phase was extracted when the synthesis reaction was terminated, and washed using the MC and hexane. Next, the solvents were removed, and drying under a reduced pressure was performed to obtain about 10.67 g (a yield: about 99%) of a cyclohexanecarboxylic acid-2,2-difluoro-2-sulfo-ethyl ester diphenyl-4-hydroxyphenylsulfonium salt, and a structure of the cyclohexanecarboxylic acid-2,2-difluoro-2-sulfo-ethyl ester diphenyl-4-hydroxyphenylsulfonium salt was observed by 1H-NMR (see FIG. 12):

WORKUP

后处理

  1. customa synthesis reaction (
  2. customIn this instance, a process of the synthesis reaction
  3. extractionThe organic phase was extracted when
  4. customthe synthesis reaction
  5. customwas terminated
  6. washwashed
  7. customNext, the solvents were removed
  8. customdrying under a reduced pressure