HRID643034

反应详情

EQUATION

反应方程式

HRID 643034 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

4

CONDITIONS

反应条件

温度
130 °C

PROCEDURE

实验过程

A mixture of 1,4-diiodobenzene (4.00 g, 12.1 mmol), 3-methylpyrazole (0.972 g, 12.1 mmol), 8-hydroxyquinoline (0.176 g, 1.21 mmol) and K2CO3 (1.69 g, 12.2 mmol) in DMSO (12 mL) was degassed before being charged with CuI (0.230 g, 1.21 mmol). The mixture in a sealed tube was heated at 130° C. overnight. Water and EtOAc were added. The mixture was filtered. The organic layer was separated, then purified by silica gel column chromatography with hexane followed by 4-6% EtOAc in hexane to give 1-(4-iodophenyl)-3-methyl-1H-pyrazole (0.98 g).

WORKUP

后处理

  1. customwas degassed
  2. filtrationThe mixture was filtered
  3. customThe organic layer was separated
  4. custompurified by silica gel column chromatography with hexane