반응 #2358559

ord-0ae59f7f6f4c4475ac094b14db351635

반응 방정식

Cn1c2ccc(S(=O)(=O)Cl)cc2c(=O)c2cc(S(=O)(=O)Cl)ccc21
10-methyl-9-oxo-9,10-dihydroacridine-2,7-disulfonyl dichloride
CC1CNCC(C)C1
3,5-dimethylpiperidine
CC1CC(C)CN(S(=O)(=O)c2ccc3c(c2)c(=O)c2cc(S(=O)(=O)N4CC(C)CC(C)C4)ccc2n3C)C1
2,7-bis(3,5-dimethylpiperidin-1-ylsulfonyl)-10-methylacridin-9(10H)-one

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: US09120754B2uspto-grants-2015_09