HRID1753668

反应详情

EQUATION

反应方程式

HRID 1753668 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a Grignard reagent prepared from 79 g of 1-bromo-4-fluorobenzene, 47 g of bis(4-tert-butylphenyl) sulfoxide obtained in Synthesis Example 1-2 and 150 g of methylene chloride were added. Under ice cooling, 49 g of trimethylsilyl chloride was added dropwise. The reaction solution was aged for 30 minutes, after which 105 g of 5 wt % dilute hydrochloric acid was added dropwise to quench the reaction. The organic layer was separated and concentrated in vacuum. Diisopropyl ether was added to the concentrate for recrystallization. The resulting crystals were collected by filtration and dried in vacuum, obtaining 68 g of the target compound, bis(4-tert-butylphenyl)(4-fluorophenyl)sulfonium bromide as white crystals. Yield 96%.

WORKUP

后处理

  1. additionwere added
  2. customto quench
  3. customthe reaction
  4. customThe organic layer was separated
  5. concentrationconcentrated in vacuum
  6. additionDiisopropyl ether was added to the
  7. concentrationconcentrate for recrystallization
  8. filtrationThe resulting crystals were collected by filtration
  9. customdried in vacuum