HRID904841

反应详情

EQUATION

反应方程式

HRID 904841 的结构方程式

PROCEDURE

实验过程

To 10 ml of 4 N hydrochloric acid containing 0.86 ml of acetic acid was added 2.22 g. of 2-amino-4-chloro-5-sulfamylaniline (VI) and the mixture refluxed for four hours. Concentration in vacuo gave a blue solid which was collected by filtration, dissolved in methanol, treated with charcoal and filtered. The blue solution was concentrated in vacuo and triturated with ether to yield a blue solid. Washing with methanol provided the product as light blue crystals which upon drying gave 1.0 g. of 5(6)-chloro-2-methyl-6(5)-sulfamyl-1(3)H-benzimidazole hydrochloride, m.p. 313°-316° C.

WORKUP

后处理

  1. concentrationConcentration in vacuo
  2. customgave a blue solid which
  3. filtrationwas collected by filtration
  4. dissolutiondissolved in methanol
  5. additiontreated with charcoal
  6. filtrationfiltered
  7. concentrationThe blue solution was concentrated in vacuo
  8. customtriturated with ether
  9. customto yield a blue solid
  10. washWashing with methanol