HRID904847
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
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
- temperaturethe suspension refluxed for 6 hours
- concentrationConcentration in vacuo
- customprovided a solid which
- additionwas then slowly added
- customAfter collecting the solid
- filtrationby filtration
- additionthe precipitate was added to 400 ml of methanol
- additionCharcoal was then added
- filtrationthe mixture filtered
- filtrationthrough filter paper
- temperaturecooled
- filtrationfiltered through Celite
- concentrationConcentration in vacuo
- customgave brown crystals which
- customupon recrystallization from acetonitrile