반응 #1354501

ord-d78d6153f26742858d93d3a002883c3d

용매

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    온도under reflux
  2. 2
    농축The reaction mixture was concentrated
  3. 3
    온도under reflux to about ⅓ of the initial volume
  4. 4
    추출The concentrate was subjected to extraction with ethyl acetate
  5. 5
    여과Resulting crystalline precipitate was collected by filtration

실험 절차

A mixture of 4-(5-methyl-2-phenyl-4-oxazolylmethoxy)benzaldehyde (2.9 g), sodium pyruvate (3.3 g), sodium carbonate (3.2 g), water (80 ml) and methanol (80 ml) was stirred for 6 hours under reflux. The reaction mixture was concentrated under reflux to about ⅓ of the initial volume. The concentrate was subjected to extraction with ethyl acetate. The aqueous layer was acidified with conc. HCl. Resulting crystalline precipitate was collected by filtration to obtain (E)-4-(5-methyl-2-phenyl-4-oxazolylmethoxy)benzylidenepyruvic acid (1.6 g, 44%). Recrystallization from chloroform-methanol gave colorless needles, m.p.197-198° C.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US06552058B1uspto-grants-2003_04