반응 #90252

ord-cec6d26d3d2a41c4af2ff2d5cd988d37

용매

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    기타Solvent was evaporated
  2. 2
    workup.ADDITIONthe residue was treated with 1 N HCl (50 mL)
  3. 3
    workup.STIRRINGstirred for 10 minutes
  4. 4
    여과Yellow product was collected by filtration
  5. 5
    세척washed with water and methanol
  6. 6
    기타dried
  7. 7
    기타Crude material was crystallized from chloroform-ethanol
  8. 8
    기타to provide 900 mg (80%) of yellow 11-4

실험 절차

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+).

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US09446021B2uspto-grants-2016_09