反応 #4658

ord-fd0d21daeb32407586c452e4c390cba8

反応条件

温度
80°CELSIUS
詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    workup.WAITleft
  2. 2
    温度to cool
  3. 3
    workup.WAITleft
  4. 4
    温度to cool
  5. 5
    その他the precipitate formed
  6. 6
    ろ過is filtered off
  7. 7
    洗浄washed with water
  8. 8
    その他recrystallized from ethanol

実験手順

A mixture of 3.6 g (0.012 mol) of ethyl 6-fluoro-7-(pyrrol-1-yl)-4-hydroxyquinoline-3-carboxylate and 4.15 g (0.03 mol) of potassium carbonate in 30 ml of dimethlformamide is heated for 30 minutes at 80° C. and left to cool, 8 g (0.06 mol) of cyclopropylmethyl bromide are added, the mixture is kept for 12 hours at 90° C. and left to cool, 80 ml of a water/ice mixture are added and the precipitate formed is filtered off, washed with water and recrystallized from ethanol to give 2.65 g of a solid melting at 125°-127° C.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US04727080uspto-grants-1988_02