HRID478657

反应详情

EQUATION

反应方程式

HRID 478657 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of 4-(3-oxo-1,4-dihydro-3H-thiochromeno[4,3-c]pyrazol-2-yl)-benzonitrile (0.100 g, 0.33 mmol) in DMSO (2 ml) was stirred vigorously at room temperature and air was flushed over the solution. After 48 h the precipitation was filtered, washed with toluen and dried. The crude product recrystallized from toluene to yield 4-(3-oxo-3H-thiochromeno[4,3-c]pyrazol-2-yl)-benzonitrile (0.036 g): 1H NMR (400 MHz, CDCl3) δ 8.65 (1H, s), 8.53 (1H, d), 8.38 (2H, d), 7.72 (2H, d), 7.66 (2H, t), 7.58-7.62 (1H, m); ESI MS m/z 304 (M+H+).

WORKUP

后处理

  1. customair was flushed over the solution
  2. customAfter 48 h the precipitation
  3. filtrationwas filtered
  4. washwashed with toluen
  5. customdried
  6. customThe crude product recrystallized from toluene