HRID1376374
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
A mixture of 1,4,5-triphenyl-3-(7-bromoheptyl)-imidazol-2-one (1.0 g) and triethyl phosphite (1.66 g) was heated at reflux temperature in xylene (5 ml) for 40 hours. The solution was evaporated to an oil and re-evaporated from ethanol. The oil was partitioned between ether and water, the ether solution was separated, dried over magnesium sulphate and evaporated to an oil which was chromatographed on silica gel (ethyl acetate) to give diethyl 7-(1,4,5-triphenylimidazol-2-yl-oxy)heptanephosphonate as an oil which solidified on standing to a white solid (0.83 g; 75%), m.p. 76°-7° C. Found: C, 70.49; H, 7.40; N, 4.94%; C32H39N204P; Requires: C, 70.31; H, 7.19; N, 5.12%.
WORKUP
后处理
- temperaturewas heated
- customThe solution was evaporated to an oil
- customre-evaporated from ethanol
- customThe oil was partitioned between ether and water
- customthe ether solution was separated
- dry with materialdried over magnesium sulphate
- customevaporated to an oil which
- customwas chromatographed on silica gel (ethyl acetate)