HRID34100

反应详情

EQUATION

反应方程式

HRID 34100 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
100 °C

PROCEDURE

实验过程

Under nitrogen atmosphere, 1 g of 6-fluoro-3-iodo-5-nitro-1-trityl-1H-indazole was dissolved in 10 mL of acetonitrile, added successively with 1.35 g of 5-vinyl-benzo[1,3]dioxole, 81.7 mg of palladium acetate (II), 162 mg of 2-(di-tert-butylphosphino)biphenyl and 2 mL of triethylamine, and stirred at 100° C. for 5 hours. After cooling to room temperature, 5 g of silica gel was added, and the solvent was evaporated, and purified by silica gel column chromatography, to obtain 468 mg of the crude product as yellow crystal. This crude product was washed with 50% diethylether solution in hexane, and the solvent was evaporated, to afford 143 mg of the title compound as yellow crystals.

WORKUP

后处理

  1. temperatureAfter cooling to room temperature
  2. addition5 g of silica gel was added
  3. customthe solvent was evaporated
  4. custompurified by silica gel column chromatography
  5. customto obtain 468 mg of the crude product as yellow crystal
  6. washThis crude product was washed with 50% diethylether solution in hexane
  7. customthe solvent was evaporated