HRID735167

反应详情

EQUATION

反应方程式

HRID 735167 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
0 °C

PROCEDURE

实验过程

38.81 mL (0.354 mmol) of trimethylorthoformate is added to a suspension of 25 g (0.141 mol) of (E)-3-(4-formylphenyl)acrylic acid in 350 mL of methanol and the mixture is refluxed for 48 hours. After cooling, the reaction mixture is filtered and the filtrate is evaporated down. The residue is taken up in 500 mL of dichloromethane and filtered through CELITE® filter aid. The filtrate is evaporated down to 150 mL and cooled to 0° C. The precipitate formed is filtered off, washed with dichloromethane/petroleum ether (1:1), and dried at 60° C. in the circulating air dryer. Yield: 12.05 g (31.5% of theory); C12H14O4 (M=222.24); calc.: molecular ion peak (M+H)+: 245; found: molecular ion peak (M+H)+: 245; Rf value: 0.6 (silica gel, petroleum ether/ethyl acetate (1:1)).

WORKUP

后处理

  1. temperaturethe mixture is refluxed for 48 hours
  2. temperatureAfter cooling
  3. filtrationthe reaction mixture is filtered
  4. customthe filtrate is evaporated down
  5. filtrationfiltered through CELITE®
  6. filtrationfilter aid
  7. customThe filtrate is evaporated down to 150 mL
  8. customThe precipitate formed
  9. filtrationis filtered off
  10. washwashed with dichloromethane/petroleum ether (1:1)
  11. customdried at 60° C. in the circulating air dryer