HRID1073686
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 solution of 19.02 g. of benzoylthiourea and 19.12 g. of ethyl bromopyruvate in 300 ml. of ethanol was refluxed for 2 hours. The solvent was removed in vacuo and the residue partitioned between ethyl acetate (1 liter) and 20% aqueous sodium carbonate (400 ml.). The organic layer was separated, washed successively with 20% aqueous sodium carbonate (3×400 ml.), water (2×400 ml.) and a brine solution (2×400 ml.) and dried over sodium sulfate. The solution was concentrated to about 50 ml. and the precipitated solids filtered and dried, 20.16 g., m.p. 146-147° C.
WORKUP
后处理
- customThe solvent was removed in vacuo
- customthe residue partitioned between ethyl acetate (1 liter) and 20% aqueous sodium carbonate (400 ml.)
- customThe organic layer was separated
- washwashed successively with 20% aqueous sodium carbonate (3×400 ml.), water (2×400 ml.)
- dry with materiala brine solution (2×400 ml.) and dried over sodium sulfate
- concentrationThe solution was concentrated to about 50 ml
- filtrationand the precipitated solids filtered
- customdried