تفاعل #1249

ord-d9ea025a9a0a4f688e80e240ea0b34ac

معادلة التفاعل

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

الكواشف

لا شيء

المذيبات

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

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

الإجراء التجريبي

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.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US05723608uspto-grants-1998_03