反应 #452426

ord-9b1f852a20544f969f0f2f8380e9970a

反应条件

温度
100°CELSIUS
详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    温度The reaction mixture was then cooled to ambient and
  2. 2
    浓缩then concentrated under reduced pressure
  3. 3
    其他The residue was partitioned between water and dichloromethane
  4. 4
    洗涤The organic phase was then washed with water
  5. 5
    干燥was then dried over sodium sulfate
  6. 6
    浓缩The remaining organics were concentrated under reduced pressure

实验过程

To a solution of 1.0 gm (9.0 mMol) 2-(4-pyrazolyl)-1-ethanol in 36 mL dimethylformamide were added 2.38 gm (22.5 mMol) sodium carbonate followed by the dropwise addition of a solution of 0.89 mL (9.0 mMol) 2-iodopropane in 8 mL dimethylformamide. The reaction mixture was heated to 100° C. for 18 hours. The reaction mixture was then cooled to ambient and then concentrated under reduced pressure. The residue was partitioned between water and dichloromethane. The organic phase was then washed with water followed by saturated aqueous sodium chloride and was then dried over sodium sulfate. The remaining organics were concentrated under reduced pressure to give 0.36 gm (26.0%) of the title compound as a brown oil.

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US06126932uspto-grants-2000_10