تفاعل #1119227

ord-ac933bc6cd32455ba1de8f8a9b506ecf

المتفاعلات

الكواشف

لا شيء

المذيبات

ظروف التفاعل

درجة الحرارة
0°CELSIUS
الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    workup.WAITThe solution was aged twenty-four hours at 20° C.
  2. 2
    درجة الحرارةwhile maintaining a temperature of 0° C
  3. 3
    استخلاصThe 4-(p-methoxyphenyl)-2-oxo-3-butenoic acid product was then extracted with 500 ml ethyl acetate
  4. 4
    أخرىisolated as a yellow solid by concentration under vacuum
  5. 5
    أخرىThe yield by HPLC analysis

الإجراء التجريبي

Sodium pyruvate (24.2 g, 0.22 mol) was dissolved in 200 ml 1N aqueous sodium hydroxide at 20° C. To this solution there was added anisaldehyde (27.4 g, 0.20 mol) at 0.2 ml/min. The solution was aged twenty-four hours at 20° C., cooled at 0° C. and acidified with 6N NCl to pH 1.0 while maintaining a temperature of 0° C. The 4-(p-methoxyphenyl)-2-oxo-3-butenoic acid product was then extracted with 500 ml ethyl acetate and isolated as a yellow solid by concentration under vacuum. The yield by HPLC analysis was 88%.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US04956490uspto-grants-1990_09