반응 #1249

ord-d9ea025a9a0a4f688e80e240ea0b34ac

반응 방정식

CCOC(=O)C(=O)CC(=O)c1c(C)cc(C)cc1C
product
CCOC(=O)C(=O)CC(=O)c1c(C)cc(C)cc1C
Ethyl 2,4-dioxo-4-(2,4,6-trimethylphenyl)butanoate
Cl
HCl
O=N[O-].[Na+]
NaNO2
CCOC(=O)C(=O)C(=NO)C(=O)c1c(C)cc(C)cc1C
semi-solid
CCOC(=O)C(=O)C(=NO)C(=O)c1c(C)cc(C)cc1C
Ethyl 2,4-dioxo-3-oximino-4-(2,4,6-trimethylphenyl)butanoate

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 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.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US05723608uspto-grants-1998_03