HRID1828120

反应详情

EQUATION

反应方程式

HRID 1828120 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
77.5 °C

PROCEDURE

实验过程

An unsubstituted metallic phthalocyanine compound is added by small portions in three times to ten times amount (by weight) of chlorosulfonic acid while maintaining at 18° C. or less. After stirring at that temperature for 1 hour, the temperature is increased at a rate of 0.5 to 1° C. per minute, and the mixture is reacted at a temperature of 130 to 135° C. for from 4 to 6 hours. Thereafter, the mixture was cooled to 70 to 85° C., thionyl chloride in an amount of twice to six times the amount of the unsubstituted metallic phthalocyanine is added dropwise while maintaining at from 70 to 80° C. over 10 to 15 hours. After stirring for several hours at that temperature, the mixture was cooled to 15 to 20° C. and continuously stirred for from 10 to 15 hours. The reaction mixture is discharged by small portions into iced water in an amount of 50 times to 200 times the amount of the metallic phthalocyanine. The resulting deposit is filtrated and washed with iced water until becoming neutral, followed by drying, to obtain a metallic phthalocyanine sulfonylchloride.

WORKUP

后处理

  1. temperaturewhile maintaining at 18° C. or less
  2. temperaturethe temperature is increased at a rate of 0.5 to 1° C. per minute
  3. customthe mixture is reacted at a temperature of 130 to 135° C. for from 4 to 6 hours
  4. temperaturewhile maintaining at from 70 to 80° C. over 10 to 15 hours
  5. stirringAfter stirring for several hours at that temperature
  6. temperaturethe mixture was cooled to 15 to 20° C.
  7. stirringcontinuously stirred for from 10 to 15 hours
  8. filtrationThe resulting deposit is filtrated
  9. washwashed with iced water
  10. customby drying