HRID2061315

反应详情

EQUATION

反应方程式

HRID 2061315 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Bis(4-tert-butylphenyl)iodonium hydrogen sulfate (0.02 mole equivalent) prepared in Synthesis Example 1-6, 0.024 mole equivalent of the aqueous solution of sodium 3,3,3-trifluoro-2-hydroxy-2-trifluoromethylpropane-1-sulfonate prepared in Synthesis Example 1-9, and 70 g of methylene chloride were mixed and agitated at room temperature for 1 hour. After the agitation, the organic layer was separated, washed by water, and then concentrated under reduced pressure. The residue was recrystallized by adding diisopropyl ether, and then the obtained crystals were recovered and dried to obtain the intended bis(4-tert-butylphenyl)iodonium 3,3,3-trifluoro-2-hydroxy-2-trifluoromethylpropane-1-sulfonate (9.4 g of white crystals (yield 72%)). The structure of the intended product is shown below.

WORKUP

后处理

  1. additionwere mixed
  2. customAfter the agitation, the organic layer was separated
  3. washwashed by water
  4. concentrationconcentrated under reduced pressure
  5. customThe residue was recrystallized
  6. additionby adding diisopropyl ether
  7. customthe obtained crystals were recovered
  8. customdried