HRID2247081

反应详情

EQUATION

反应方程式

HRID 2247081 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
125 °C

PROCEDURE

实验过程

Oleum (20-25% SO3, 800 g), dimethyl terephthalate (234 g) and paraformaldehyde (48 g) are heated with stirring for 5 hours at 125° C. The reaction mixture is cooled to 70° C. and poured into ethanol (1,6 L) having room temperature. This mixture is heated to reflux for 1½ hour before ice (800 g) is added. The suspension is stirred overnight, filtered off and washed with ethanol (150 ml). The crude product is suspended in water (800 ml) and pH is adjusted to 4 with NaOH (27%). The precipitate is filtered off and washed with water and dried.

WORKUP

后处理

  1. temperatureThe reaction mixture is cooled to 70° C.
  2. customhaving room temperature
  3. temperatureThis mixture is heated
  4. additionis added
  5. stirringThe suspension is stirred overnight
  6. filtrationfiltered off
  7. washwashed with ethanol (150 ml)
  8. filtrationThe precipitate is filtered off
  9. washwashed with water
  10. customdried