HRID1484706

反应详情

EQUATION

反应方程式

HRID 1484706 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of compound N-(4-(2-chloroacetyl)-3,5-dimethylphenyl)acetamide (3.4 g, 14.2 mmol), thiourea (1.79 g, 23.6 mmol) and KI (150 mg) in toluene (50 mL) and 95% EtOH (50 mL) was refluxed overnight. After the solvent was distilled off, the residue was dissolved in EtOAc (600 mL) and washed with saturated Na2CO3 solution and brine successively, and dried over Na2SO4. After removal of solvent, the residue was subjected to column chromatography (silica gel, EtOAc:NH4OH=100:0.5) to furnish N-(4-(2-aminothiazol-4-yl)-3,5-dimethylphenyl)acetamide (3.2 g, 86.1% yield).

WORKUP

后处理

  1. distillationAfter the solvent was distilled off
  2. dissolutionthe residue was dissolved in EtOAc (600 mL)
  3. washwashed with saturated Na2CO3 solution and brine successively
  4. dry with materialdried over Na2SO4
  5. customAfter removal of solvent