HRID364647
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
CONDITIONS
反应条件
- 温度
- 130 °C
PROCEDURE
实验过程
There is prepared from 50 g triphenylphosphine and 38.5 g 1,3-dibrompropane in 150 ml xylene by heating for 20 hours at 130° C. under nitrogen 80 g crystalline (3-bromopropyl)-triphenylphosphoniumbromide with a melting point of 226° C. This is stirred using a solution of 33 g (0.7M) dimethylamine in 200 ml ethanol for 20 hours at 20°-25° C.) The residue is absorbed after removal of ethanol in a vacuum in 2-propanol and precipitated using hydrogen bromide gas. After recrystallization from ethanol, 43 g (3-dimethylaminopropyl)-triphenylphosphoniumbromide HBr is obtained with a melting point of 279° C.
WORKUP
后处理
- customfor 20 hours
- customat 20°-25° C.
- customis absorbed
- customafter removal of ethanol in a vacuum in 2-propanol
- customprecipitated
- customAfter recrystallization from ethanol