HRID57277

反应详情

EQUATION

反应方程式

HRID 57277 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

The 2-benzothiazol-2-yl-3-chloro-3-furan-2-ylacrylonitrile (480 mg, 1.7 mmol) prepared above and hydrazine hydrate (100 mg, 2 mmol) were refluxed in methanol (15 mL) for 3 hrs. The solvent was then evaporated and the residue was purified by flash column chromatography eluting with CH2Cl2:MeOH=9:1 to afford 130 mg of material. This was further purified by preparative TLC eluting with CH2Cl2:MeOH=9:1 to yield 23 mg (5%) of the title compound. MS (m/z, ES+): 283.0 (M+1, 100%).

WORKUP

后处理

  1. customThe solvent was then evaporated
  2. customthe residue was purified by flash column chromatography
  3. washeluting with CH2Cl2