HRID904847

反应详情

EQUATION

反应方程式

HRID 904847 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To 50 ml of 4 N hydrochloric acid containing 11.8 g of 2-amino-4-chloro-5-sulfamylaniline was added 9.2 g of hexanoic acid and the suspension refluxed for 6 hours. Concentration in vacuo provided a solid which was then slowly added with stirring to 100 ml of 38% ammonium hydroxide. After collecting the solid by filtration, the precipitate was added to 400 ml of methanol and the suspension brought to a boil. Charcoal was then added and the mixture filtered through filter paper, cooled, and filtered through Celite. Concentration in vacuo gave brown crystals which upon recrystallization from acetonitrile provided 2.6 g of product, mp 183°-185°.

WORKUP

后处理

  1. temperaturethe suspension refluxed for 6 hours
  2. concentrationConcentration in vacuo
  3. customprovided a solid which
  4. additionwas then slowly added
  5. customAfter collecting the solid
  6. filtrationby filtration
  7. additionthe precipitate was added to 400 ml of methanol
  8. additionCharcoal was then added
  9. filtrationthe mixture filtered
  10. filtrationthrough filter paper
  11. temperaturecooled
  12. filtrationfiltered through Celite
  13. concentrationConcentration in vacuo
  14. customgave brown crystals which
  15. customupon recrystallization from acetonitrile