반응 #446032

ord-cf512ed7d25e4c498ac10272e7521869

용매

반응 조건

온도
80°CELSIUS
상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    workup.ADDITIONThe reaction solution is then poured onto ice
  2. 2
    기타the phases are separated
  3. 3
    기타After some time the above acid crystallises out and
  4. 4
    여과is filtered off with suction
  5. 5
    기타dried

실험 절차

12 g of potassium tert.-butoxide are added to a solution of 14 g of 6-(thiophen-3-yl)-pyridine-2,3-dicarboxylic acid diethyl ester and 6 g of 2-amino-2,3-dimethyl- butyramide in 100 ml of dry toluene while stirring and the solution is heated at 80° C. for 5 hours. The reaction solution is then poured onto ice, the phases are separated and the aqueous phase is acidified with 10 ml of glacial acetic acid. After some time the above acid crystallises out and is filtered off with suction and dried. In this manner 13.5 g of 6-(thiophen-3-yl)-2-(5-isopropyl-5-methyl-4-oxo-imidazol-2-yl)-pyridine-3-carboxylic acid having a melting point of 253°-257° C. are obtained.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US04997947uspto-grants-1991_03