反应 #91658

ord-0ca8794b5619488e887182cf5776361d

反应条件

温度
120°CELSIUS
详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    其他After the completion of the reaction
  2. 2
    过滤the reaction mixture was filtered
  3. 3
    workup.ADDITIONThe filtrate was added with water
  4. 4
    萃取extracted with ethyl acetate
  5. 5
    干燥The obtained organic layer was dried over magnesium sulfate
  6. 6
    其他purified by column chromatography (ethyl acetate:hexane=1:3)

实验过程

2-Bromopyridin-3-ol (100 mg, 0.58 mmol), 3-thiophenyl boronic acid (88 mg, 0.69 mmol), sodium carbonate (184 mg, 2.07 mmol) and Pd2(dppf)2Cl2 (94 mg, 0.12 mmol) were dissolved in dimethoxyethane/water of 1 mL/1 mL, followed by stirring in microwave at 120° C. for 20 minutes. After the completion of the reaction, the reaction mixture was filtered using Celite. The filtrate was added with water, and extracted with ethyl acetate. The obtained organic layer was dried over magnesium sulfate, and purified by column chromatography (ethyl acetate:hexane=1:3) to obtain 2-(thiophene-3-yl)pyridin-3-ol (50 mg, 48%).

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US09447083B2uspto-grants-2016_09