반응 #1119224

ord-7afc625aec9e40b288fe40525353d684

용매

반응 조건

온도
20°CELSIUS
상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    온도maintaining the temperature below 5° C
  2. 2
    workup.WAITwas aged an additional six hours
  3. 3
    기타reaction
  4. 4
    온도The mixture was cooled to -10° C.
  5. 5
    추출The p-chlorobenzalpyruvic acid product was then extracted with 800 mL ethyl acetate in 94% yield

실험 절차

Sodium pyruvate (24.2 g, 0.22 moL) was added to a cold (0° C.) solution of 1N sodium hydroxide (200 mL) and ethanol (10 mL). p-Chlorobenzaldehyde (28.11 g, 0.20 moL) was then added, maintaining the temperature below 5° C. The reaction mixture was aged six hours at 0°-5° C. and then allowed to warm to 20° C. where it was aged an additional six hours to effect complete reaction. The mixture was cooled to -10° C. and the pH adjusted to 1.0 with cold 6N HCl. The p-chlorobenzalpyruvic acid product was then extracted with 800 mL ethyl acetate in 94% yield.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US04956490uspto-grants-1990_09