HRID60889

反应详情

EQUATION

反应方程式

HRID 60889 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

A mixture of methyl 2-bromo-5-methylbenzoate (1.01 g, 4.41 mmol), 1-methyl-4-(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl)-1H-pyrazole (1.1 g, 5.28 mmol), Pd(PPh3)4 (0.764 g, 0.66 mmol), K2CO3 (1.83 g, 13.23 mmol) and dioxane/H2O (4:1, 15 mL) was degassed for 10 min and then heated overnight at 100° C. The mixture was cooled, diluted with brine, and extracted with EtOAc. The combined organic layers were washed with saturated NaHCO3 and dried over Na2SO4. The solvent was removed in vacuo to obtain the crude material, which was purified by silica gel chromatography to obtain the title compound. ESI-MS (m/z): 231 [M+1]+.

WORKUP

后处理

  1. customwas degassed for 10 min
  2. temperatureThe mixture was cooled
  3. additiondiluted with brine
  4. extractionextracted with EtOAc
  5. washThe combined organic layers were washed with saturated NaHCO3
  6. dry with materialdried over Na2SO4
  7. customThe solvent was removed in vacuo
  8. customto obtain the crude material, which
  9. customwas purified by silica gel chromatography