HRID902110
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
13 g of ethyl 4-methyl-2-(4-methylbenzoylamino)-3-oxopentanoate in 80 ml of phosphorus oxychloride are heated to the boil under reflux for 2 h. The phosphorus oxychloride is removed under reduced pressure and the resulting residue is dissolved in 200 ml of dichloromethane, washed three times with saturated NaHCO3 solution and dried over MgSO4, and the solvent is then removed under reduced pressure. This gives 11 g of ethyl 5-isopropyl-2-p-tolyloxazole-4-carboxylate as a brownish sold. C16H19NO3 (273.33), MS(ESI)=292 (M+H+), Rf(n-heptane:ethyl acetate)=2:1)=0.43.
WORKUP
后处理
- temperatureunder reflux for 2 h
- customThe phosphorus oxychloride is removed under reduced pressure
- dissolutionthe resulting residue is dissolved in 200 ml of dichloromethane
- washwashed three times with saturated NaHCO3 solution
- dry with materialdried over MgSO4
- customthe solvent is then removed under reduced pressure