反应 #1249

ord-d9ea025a9a0a4f688e80e240ea0b34ac

溶剂

反应条件

详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    其他The solvent was removed from the mixture and 200 mL of water
  2. 2
    workup.ADDITIONwas added to the residue
  3. 3
    萃取The product was then extracted into ether
  4. 4
    萃取The ether extract
  5. 5
    干燥was dried over Na2SO4
  6. 6
    其他evaporated

实验过程

N2O3 gas was slowly passed into a stirred solution of the product of step A (16.2 g) in 300 mL of ethanol until the disappearance of starting material was confirmed by TLC. N2O3 gas was generated by the dropwise addition of 12N aqueous HCl solution into an aqueous slurry of NaNO2. The solvent was removed from the mixture and 200 mL of water was added to the residue. The product was then extracted into ether. The ether extract was dried over Na2SO4 and evaporated to give 16.1 g of a semi-solid.

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US05723608uspto-grants-1998_03