反応 #52217

ord-d327b4f511f44069aecb5e4b9549be84

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    洗浄the solution was washed with 5% NaHCO3 (2×50 ml)
  2. 2
    乾燥dried over Na2SO4
  3. 3
    ろ過The solution was filtered
  4. 4
    その他evaporated under vacuum to dryness
  5. 5
    その他The residue was crystallized from hexane-CHCl3

実験手順

Morpholine (1.9 ml; 21.8 mmol) was added to a solution of 5-chloromethyl-8-hydroxyquinoline (1.98 g; 8.34 mmol) in CHCl3 (50 ml) at 5° C. The reaction mixture was stirred overnight at room temperature. Then CHCl3 (100 ml) was added and the solution was washed with 5% NaHCO3 (2×50 ml), followed by brine (50 ml), and dried over Na2SO4. The solution was filtered and evaporated under vacuum to dryness. The residue was crystallized from hexane-CHCl3 and gave 1.2 g (59%) of the title product. M.p. 130° C. TLC (CHCl3; MeOH; NH3=8:2:0.5. Rf=0.69.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US06855711B1uspto-grants-2005_02