反応 #2358559

ord-0ae59f7f6f4c4475ac094b14db351635

溶媒

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    その他Solvent was evaporated
  2. 2
    workup.ADDITIONthe residue was treated with 1 N HCl (50 mL)
  3. 3
    workup.STIRRINGstirred for 10 minutes
  4. 4
    ろ過Yellow product was collected by filtration
  5. 5
    洗浄washed with water and methanol
  6. 6
    その他dried
  7. 7
    その他Crude material was crystallized from chloroform-ethanol
  8. 8
    その他to provide 900 mg (80%) of yellow 11-4

実験手順

To a solution of 10-methyl-9-oxo-9,10-dihydroacridine-2,7-disulfonyl dichloride from Example 7 (810 mg, 2 mmole) in THF (20 mL) was added 3,5-dimethylpiperidine (2 mL, 15 mmole) and the reaction mixture was stirred at room temperature for 6 hours. Solvent was evaporated and the residue was treated with 1 N HCl (50 mL) and stirred for 10 minutes. Yellow product was collected by filtration, washed with water and methanol and dried. Crude material was crystallized from chloroform-ethanol to provide 900 mg (80%) of yellow 11-4. MS 560 (MH+).

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US09120754B2uspto-grants-2015_09