HRID1295258

反应详情

EQUATION

反应方程式

HRID 1295258 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of methyl 4-bromo-5-oxo-5-phenylpentanoate (15.0 g), thiourea (3.81 g) and methanol (200 ml) was refluxed for 2 hrs. The reaction solvent was removed under reduced pressure, and the residue was dissolved in ethyl acetate. The obtained solution was washed successively with saturated aqueous sodium hydrogen carbonate and saturated brine, dried over anhydrous magnesium sulfate and concentrated to give methyl 3-(2-amino-4-phenyl-5-thiazolyl)propionate (11.9 g, yield 90%) as pale-yellow crystals. The crystals were recrystallized from ethyl acetate-hexane. melting point: 130–131° C.

WORKUP

后处理

  1. temperaturewas refluxed for 2 hrs
  2. customThe reaction solvent was removed under reduced pressure
  3. dissolutionthe residue was dissolved in ethyl acetate
  4. washThe obtained solution was washed successively with saturated aqueous sodium hydrogen carbonate and saturated brine
  5. dry with materialdried over anhydrous magnesium sulfate
  6. concentrationconcentrated