HRID378259

反应详情

EQUATION

反应方程式

HRID 378259 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

0.98 g (0.006 mol) of 2-amino-4,6-dichloropyrimidine and 3.03 g (0.012 mol) of N-(4-sulfamoyl-phenyl)-acetamide potassium salt were stirred in 10 ml of 1-methyl-2-pyrrolidone at 140° C. for 8 hours. Then, the solvent was distilled off in a high vacuum, the residue was partitioned in ethyl acetate/water, the inorganic phase was saturated with sodium chloride and the remaining ethyl acetate dissolved in the aqueous was distilled off on a rotary evaporator. The aqueous phase was made acid with 1N HCl, the crystals which separated were filtered off under section and washed with water. After drying there were obtained 1.37 g (67%) of N-[4-(2-amino-6-chloro-pyrimidin-4-yisulfamoyl)-phenyl]-acetamide as beige crystals; m.p.: 272-273° C. (dec.).

WORKUP

后处理

  1. distillationThen, the solvent was distilled off in a high vacuum
  2. customthe residue was partitioned in ethyl acetate/water
  3. dissolutionthe remaining ethyl acetate dissolved in the
  4. distillationaqueous was distilled off on a rotary evaporator
  5. customthe crystals which separated
  6. filtrationwere filtered off under section
  7. washwashed with water
  8. customAfter drying there