HRID2261640

反应详情

EQUATION

反应方程式

HRID 2261640 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

To a suspension of 2-(1-cyano-2-methoxypropenyl)benzothiazole-5-sulfonic acid methylamide (120 mg, 0.37 mmol) in 4 mL of methanol, was added hydrazine hydrate (20 μL). The mixture was heated to reflux for 5 hrs and then 1 drop of conc. hydrochloric acid was added to the reaction mixture. The mixture was refluxed for an additional 5 min and was then allowed to cool. The volume of solvent was reduced under reduced pressure and a solid formed. The solid was isolated by filtration and was washed with methanol and then water and dried to yield 51 mg (43%) of the title compound as a cream coloured powder. MS (m/z, ES+): 324.0 (M+1, 100%).

WORKUP

后处理

  1. temperatureThe mixture was heated
  2. temperatureto reflux for 5 hrs
  3. temperatureThe mixture was refluxed for an additional 5 min
  4. temperatureto cool
  5. customa solid formed
  6. customThe solid was isolated by filtration
  7. washwas washed with methanol
  8. dry with materialwater and dried