HRID1413120
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
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
- temperatureThe mixture was heated
- temperatureunder reflux for one hour
- distillationExcess thionyl chloride and benzene were distilled off
- distillationthe residue was fractionally distilled
- customA fraction boiling at 105° to 108° C. (2 mm Hg) was collected