반응 #1353334

ord-12da3de273734e1aa40c4bcd66fd269e

용매

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    기타The solvent was removed from the mixture and 200 mL of water
  2. 2
    workup.ADDITIONwas added to the residue
  3. 3
    추출The product was then extracted into ether
  4. 4
    추출The ether extract
  5. 5
    건조was dried over Na2SO4
  6. 6
    기타evaporated

실험 절차

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 12 N 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.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US06548509B2uspto-grants-2003_04