HRID610792

反应详情

EQUATION

反应方程式

HRID 610792 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

2.7 g (0.008 mol) of N-[4-(6-chloro-2-methylamino-pyrimidin-4-ylsulfamoyl)-phenyl]-acetamide were dissolved in 76 ml of 1N NaOH and boiled at reflux for 3 hours. The mixture was extracted with ethyl acetate, the aqueous phase was saturated with sodium chloride and the residual ethyl acetate was distilled off on a rotary evaporator. Then, the aqueous phase was made acid with 3N HCl and the precipitate which separated was filtered off under suction. After drying there were obtained 2.12 g (89%) of 4-amino-N-(6-chloro-2-methylamino-pyrimidin-4-yl)-benzenesulfonamide hydrochloride (1:1.9) as white crystals; MS (ISN): me/e=312 (C11H11ClN5O2S-).

WORKUP

后处理

  1. temperatureat reflux for 3 hours
  2. extractionThe mixture was extracted with ethyl acetate
  3. distillationthe residual ethyl acetate was distilled off on a rotary evaporator
  4. customthe precipitate which separated
  5. filtrationwas filtered off under suction
  6. customAfter drying there