HRID64686

反应详情

EQUATION

反应方程式

HRID 64686 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

4 Grams (0.021 mole) of 3-carboxymethylrhodanine was dissolved into 30 ml of acetic acid. To the solution were added 2 g (0.021 mole) of hexa-2,4-dienal and 3.8 g (0.046 mole) of sodium acetate, and the resultant was stirred under mild reflux for 5 hours. The obtained black reaction mixture was concentrated to about one-half its initial volume under reduced pressure. The residual mixture was poured into water to form precipitate. The precipitate was extracted with ethyl acetate and the extract was recrystallized from a mixed solvent of methylene chloride and ethyl acetate to give 4.1 g of 3-carboxymethyl-5-(2,4-hexadienylidene)rhodanine in the form of yellow prism (yield: 73%).

WORKUP

后处理

  1. temperatureunder mild reflux for 5 hours
  2. concentrationThe obtained black reaction mixture was concentrated to about one-half its initial volume under reduced pressure
  3. additionThe residual mixture was poured into water
  4. customto form precipitate
  5. extractionThe precipitate was extracted with ethyl acetate
  6. customthe extract was recrystallized from a mixed solvent of methylene chloride and ethyl acetate