反应 #2195488

ord-fd466009186449ee86a027ef269d8b74

反应方程式

Cl
hydrochloric acid
CCN(CC)CC
Triethylamine
CC(C)(C)C(=O)OC(C(F)(F)F)C(F)(F)S(=O)(=O)[O-].[Na+]
sodium 1,1,3,3,3-pentafluoro-2-(pivaloyloxy)propanesulfonate
ClCCl
dichloromethane
CC(C)(C)C(=O)OC(C(F)(F)F)C(F)(F)S(=O)(=O)[O-].C[NH+](C)C
trimethylammonium 1,1,3,3,3-pentafluoro-2-(pivaloyloxy)propanesulfonate
收率 75.0%

溶剂

反应条件

详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    workup.ADDITIONwere added, whereupon the mixture
  2. 2
    其他The organic layer was separated
  3. 3
    洗涤washed with water
  4. 4
    洗涤From the organic layer as washed
  5. 5
    workup.DISTILLATIONthe dichloromethane was distilled off in vacuum
  6. 6
    workup.ADDITIONDiethyl ether was added to the residue for recrystallization
  7. 7
    过滤The crystals were filtered
  8. 8
    其他dried
  9. 9
    其他obtaining the target compound in a yield of 75%

实验过程

Triethylamine was dissolved in cold water. To the solution, hydrochloric acid was added, and sodium 1,1,3,3,3-pentafluoro-2-(pivaloyloxy)propanesulfonate prepared in Synthesis Example 27 and dichloromethane were added, whereupon the mixture was stirred. The organic layer was separated and washed with water. From the organic layer as washed, the dichloromethane was distilled off in vacuum. Diethyl ether was added to the residue for recrystallization. The crystals were filtered and dried, obtaining the target compound in a yield of 75%.

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US07514202B2uspto-grants-2009_04