反应 #52805

ord-65dff62d1c984259a876017f3cdcbf41

溶剂

反应条件

详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    温度was refluxed for 4 hours
  2. 2
    其他a precipitate formed
  3. 3
    温度The mixture was refluxed for 5 minutes
  4. 4
    过滤The precipitate was collected by vacuum filtration
  5. 5
    洗涤washed with 20 mL of ethanol
  6. 6
    洗涤The solids were slurry-washed in 30 mL of refluxing ethanol
  7. 7
    温度cooled
  8. 8
    过滤collected by vacuum filtration
  9. 9
    洗涤washed with 30 mL of ethanol and vacuum
  10. 10
    其他dried

实验过程

A mixture of (2-Formyl-4,5,6,7-tetrahydro-1H-indol-3-yl)-propionic acid (5.4 g), 5.0 g of 5-bromo-4-methyl-2-oxindole and 2.7 g of piperidine in 25 mL of ethanol was refluxed for 4 hours. Acetic acid (8 mL) was slowly added and a precipitate formed. The mixture was refluxed for 5 minutes and cooled to ambient temperature. The precipitate was collected by vacuum filtration and washed with 20 mL of ethanol. The solids were slurry-washed in 30 mL of refluxing ethanol, cooled, collected by vacuum filtration, washed with 30 mL of ethanol and vacuum dried to give 7.6 g (80%) of 3-[2-(5-bromo-4-methyl-2-oxo-1,2-dihydroindol-3-ylidenemethyl)-4,5,6,7-tetrahydro-1H-indol-3-yl]-propionic acid as an red-orange solid.

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US06855730B2uspto-grants-2005_02