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
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-ylsulfamoyl)-phenyl]-acetamide as beige crystals; m.p.: 272-273° C. (dec.).
WORKUP
后处理
- distillationThen, the solvent was distilled off in a high vacuum
- customthe residue was partitioned in ethyl acetate/water
- dissolutionthe remaining ethyl acetate dissolved in the
- distillationaqueous was distilled off on a rotary evaporator
- customthe crystals which separated
- filtrationwere filtered off under section
- washwashed with water
- customAfter drying there