HRID402479

反应详情

EQUATION

反应方程式

HRID 402479 的结构方程式

CONDITIONS

反应条件

温度
120 °C

PROCEDURE

实验过程

A mixture of 1-methyl-3-phenyl-4-(trifluoromethyl)-1H-pyrazolo[3,4-b]pyridin-6(7H)-one (1.0 g, 3.4 mmol) and POBr3 (0.962 g, 3.4 mmol) was heated at 120° C. for 3 h. The reaction mixture was cooled to it and poured into rapidly stirred ice cold water to obtain a solid product. The product was collected by filtration and dried under vacuum to yield an off-white solid (1.20 g, 99%). [1H-NMR (CDCl3, 300 MHz) δ 7.58 (s, 1H), 7.54-7.41 (m, 5H), 4.22 (s, 3H); LCMS RtA=1.943 min; [M+H]+=355.9]

WORKUP

后处理

  1. temperatureThe reaction mixture was cooled to it
  2. additionpoured into rapidly stirred ice cold water
  3. customto obtain a solid product
  4. filtrationThe product was collected by filtration
  5. customdried under vacuum