HRID231350
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
- 65 °C
PROCEDURE
实验过程
To a solution of 100 g (0.588 mole) of 10-undecenyl alcohol and 2 g of pyridine was added 75 g (0.63 mole) of SOCl2 dropwise over a period of 45 minutes at 25° C. The solution was heated at 65° C. for 5 hours. CH2Cl2 (100 mL) was added and the solution was water washed twice, dried with MgSO4, filtered, and the CH2Cl2 evaporated. The residue (103 g) by GC analysis showed a purity of 99.3% VIII with 0.7% alcohol; IR showed no OH band and absorbence at 1641-1. Distillation (15.24 centimeter jacketed Vigreaux column) gave 94 g VIII (bp 104°-105° C. at 6 mm) (GC showed no alcohol; 100% VIII).
WORKUP
后处理
- washwashed twice
- dry with materialdried with MgSO4
- filtrationfiltered
- customthe CH2Cl2 evaporated
- distillationDistillation (15.24 centimeter jacketed Vigreaux column)