HRID1283833
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- customa vigorous reaction
- customprecipitating
- temperatureThe mixture is then heated
- temperatureat reflux for 5 minutes
- temperatureAfter chilling
- customthe crude dye is collected on
- filtrationa filter
- washrinsed with ethanol
- customdried
- customAfter one recrystallization from methanol