HRID1073686

反应详情

EQUATION

反应方程式

HRID 1073686 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

  1. customThe solvent was removed in vacuo
  2. customthe residue partitioned between ethyl acetate (1 liter) and 20% aqueous sodium carbonate (400 ml.)
  3. customThe organic layer was separated
  4. washwashed successively with 20% aqueous sodium carbonate (3×400 ml.), water (2×400 ml.)
  5. dry with materiala brine solution (2×400 ml.) and dried over sodium sulfate
  6. concentrationThe solution was concentrated to about 50 ml
  7. filtrationand the precipitated solids filtered
  8. customdried