HRID1465758

反应详情

EQUATION

反应方程式

HRID 1465758 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
140 °C

PROCEDURE

实验过程

5-Bromo-4-methyl-2-benzofuran-1(3H)-one (598 mg, 4.47 mmol), potassium vinyl trifluoroborate (507 mg, 2.23 mmol), PdCl2(dppf)-CH2Cl2 Adduct (182 mg, 0.223 mmol), and TEA (0.622 mL, 4.47 mmol) were added to 10 mL ethanol in a 20 mL microwave tube. The tube was sealed and degassed, then heated to 140° C. for 20 min. Analysis by LC-MS showed product peak. The reaction mixture was diluted with ethyl acetate, washed with brine twice, dried and evaporated to dryness. The crude product was purified by MPLC chromatography using a 120 g Redi-sep column and 0-80% EtOAC/Hexane solvent system to yield the title product. LC-MS: M+1=175 at 2.42 retention time.

WORKUP

后处理

  1. customThe tube was sealed
  2. customdegassed
  3. additionThe reaction mixture was diluted with ethyl acetate
  4. washwashed with brine twice
  5. customdried
  6. customevaporated to dryness
  7. customThe crude product was purified by MPLC chromatography