HRID1413120

反应详情

EQUATION

反应方程式

HRID 1413120 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Into a solution of 5.5 g (0.028 mole) of tricyclo[4,3,1,12,5 ]undecane-1-carboxylic acid (IV) in 20 ml of dry benzene was added dropwise with stirring 12 ml of thionyl chloride at room temperature. The mixture was heated under reflux for one hour. Excess thionyl chloride and benzene were distilled off and the residue was fractionally distilled. A fraction boiling at 105° to 108° C. (2 mm Hg) was collected to give 5.2 g (87% yield) of 1-chlorocarbonyltricyclo[4,3,1,12,5 ]undecane. IR (neat):

WORKUP

后处理

  1. temperatureThe mixture was heated
  2. temperatureunder reflux for one hour
  3. distillationExcess thionyl chloride and benzene were distilled off
  4. distillationthe residue was fractionally distilled
  5. customA fraction boiling at 105° to 108° C. (2 mm Hg) was collected