HRID2061304

反应详情

EQUATION

反应方程式

HRID 2061304 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

About 10 g of the diphenyl-4-hydroxyphenylsulfonium trifluoromethanesulfonate salt manufactured in the synthesis example 3 and about 9.7 g of an adamantane-1-carboxylic 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 11 below) was performed while strongly stirring for 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 of a soluble solvent and hexane of a sparingly soluble solvent. Next, the solvents were removed, and drying under a reduced pressure was performed to obtain about 11.47 g (a yield: about 81.7%) of an adamantane-1-carboxylic acid-2,2-difluoro-2-sulfo-ethyl ester diphenyl-4-hydroxyphenylsulfonium salt, and a structure of the adamantane-1-carboxylic acid-2,2-difluoro-2-sulfo-ethyl ester diphenyl-4-hydroxyphenylsulfonium salt was observed by 1H-NMR (see FIG. 10):

WORKUP

后处理

  1. customa synthesis reaction (see Equation 11 below)
  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