HRID1283837

反应详情

EQUATION

反应方程式

HRID 1283837 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)-pyrrolidinium perchlorate (3.2 g.), dodecylsulfonylacetonitrile (2.7 g.) and triethylamine (3.1 ml.) are dissolved in ethanol (15 ml.) and heated at reflux for 5 minutes. After chilling, the solid is collected on a filter, washed with methanol and dried. Obtaining pure dye by recrystallization from methanol proved difficult. The product is eluted from basic alumina, using a 10% methanol-90% chloroform solvent mixture, and then recrystallized from methanol. The yield of purified dye is 0.5 g. (11%), m.p. 114°-115°C. This dye compound shows good ultraviolet absorption characteristics as indicated in the data in Table 1 below.

WORKUP

后处理

  1. temperatureheated
  2. temperatureat reflux for 5 minutes
  3. temperatureAfter chilling
  4. customthe solid is collected on a filter
  5. washwashed with methanol
  6. customdried
  7. customObtaining pure dye
  8. customby recrystallization from methanol proved difficult
  9. washThe product is eluted from basic alumina
  10. customrecrystallized from methanol
  11. customultraviolet absorption characteristics