HRID1077305

反应详情

EQUATION

反应方程式

HRID 1077305 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 2-butyrylfluorene (11.3 g.), powdered potassium hydroxide (4.16 g.) and 100% hydrazine hydrate (9 ml.) in ethylene glycol (104 ml.) was refluxed for one hour with stirring. The mixture was then slowly distilled until the boiling-point reached 185° and then heated to reflux for 3 hours. The cooled mixture was treated with water (ca. 300 ml.) and the produce was isolated with ether in the usual manner. Recrystallisation from methanol gave 2-butyfluorene, m.p. 65°-66.5° .

WORKUP

后处理

  1. temperaturewas refluxed for one hour
  2. distillationThe mixture was then slowly distilled until the boiling-point
  3. customreached 185°
  4. temperatureheated
  5. temperatureto reflux for 3 hours
  6. additionThe cooled mixture was treated with water (ca. 300 ml.)
  7. customthe produce was isolated with ether in the usual manner
  8. customRecrystallisation from methanol