HRID1281110

反应详情

EQUATION

反应方程式

HRID 1281110 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a mixture of terephthalaldehyde mono-(diethyl acetal) (3.96 mL, 20.0 mmol) and 2,4-thiazolidinedione (2.81 g, 24.0 mmol) in ethanol (40 mL) was added piperidine (2.0 mL, 20.0 mmol). The reaction mixture was heated to reflux for 4 h. After cooling on an ice-bath, hydrochloric acid (0.2 mol/L, 100 mL) was added and the precipitated products were collected by filtration. The cake was washed with water and dried. To a solution of this product (5.50 g) in tetrahydrofuran (180 mL) was added hydrochloric acid (1 mol/L, 18 mL) and the mixture was stirred at room temperature for 2 h. Water was added, and the precipitated products were collected by filtration to give 5-(4-formylbenzylidene)-2,4-thiazolidinedione (3.91 g, 94%).

WORKUP

后处理

  1. temperatureThe reaction mixture was heated
  2. temperatureto reflux for 4 h
  3. temperatureAfter cooling on an ice-bath
  4. filtrationthe precipitated products were collected by filtration
  5. washThe cake was washed with water
  6. customdried
  7. additionTo a solution of this product (5.50 g) in tetrahydrofuran (180 mL) was added hydrochloric acid (1 mol/L, 18 mL)
  8. additionWater was added
  9. filtrationthe precipitated products were collected by filtration