HRID1283833

反应详情

EQUATION

反应方程式

HRID 1283833 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

N-(3-Chloro-5,5-dimethylcyclohex-2-en-1-ylidene)-pyrrolidiniumperchlorate (9.4 g., 0.03 mol.) and malononitrile (2.0 g., 0.03 mol.) are dissolved in warm ethanol (25 ml.). Triethylamine (4.6 ml.) is then added and a vigorous reaction takes place with a solid precipitating. The mixture is then heated at reflux for 5 minutes. After chilling, the crude dye is collected on a filter and rinsed with ethanol and dried. After one recrystallization from methanol, the yield of purified dye is 3.0 g. (83%), m.p. 246°-247°C. This purified dye is an excellent light-absorbing dye in photographic layers as shown in the absorption data in Table 1 hereinafter.

WORKUP

后处理

  1. customa vigorous reaction
  2. customprecipitating
  3. temperatureThe mixture is then heated
  4. temperatureat reflux for 5 minutes
  5. temperatureAfter chilling
  6. customthe crude dye is collected on
  7. filtrationa filter
  8. washrinsed with ethanol
  9. customdried
  10. customAfter one recrystallization from methanol