HCID 66714108, compound → HCID 56645391, compound

HRID 876877Notes

Reaction equation

HRID 876877 reaction equation
C(OC(=O)[NH:7][C:8]1([C:12]2[CH:17]=[CH:16][C:15]([C:18]3[C:19]([C:35]4[CH:40]=[CH:39][CH:38]=[CH:37][CH:36]=4)=[CH:20][C:21]4[N:22]([C:24]([C:28]5[CH:33]=[CH:32][C:31]([F:34])=[CH:30][CH:29]=5)=[C:25]([Cl:27])[N:26]=4)[N:23]=3)=[CH:14][CH:13]=2)[CH2:11][CH2:10][CH2:9]1)(C)(C)C>Cl.O1CCOCC1>[Cl:27][C:25]1[N:26]=[C:21]2[CH:20]=[C:19]([C:35]3[CH:40]=[CH:39][CH:38]=[CH:37][CH:36]=3)[C:18]([C:15]3[CH:14]=[CH:13][C:12]([C:8]4([NH2:7])[CH2:11][CH2:10][CH2:9]4)=[CH:17][CH:16]=3)=[N:23][N:22]2[C:24]=1[C:28]1[CH:29]=[CH:30][C:31]([F:34])=[CH:32][CH:33]=1

Participants

4

Reactant 1

HCID 66714108HCID 66714108, compound

Product 1

HCID 56645391HCID 56645391, compound

Reagents, catalysts & solvents 2

HCID 313Hydrochloric AcidSolventHCID 312751,4-DioxaneSolvent

Procedure

12.1 mg (0.98 mmol) (1-{4-[2-Chloro-3-(4-fluorophenyl)-7-phenyl-imidazo[1,2-b]pyridazin-6-yl]-phenyl}-cyclobutyl)-carbamic acid tert-butyl ester in 1 mL 4M hydrogen chloride in dioxane were stirred over night at room temperature. After evaporation of the solvent the residue was dissolved in methanol and given on a ForaPak Rxn CX column. The column was washed with 100 mL methanol and the product was eluted with methanol/NH3 yielding 9.8 mg (93.4%) of the title compound.

Workup

  1. customAfter evaporation of the solvent the residue
  2. dissolutionwas dissolved in methanol
  3. washThe column was washed with 100 mL methanol
  4. washthe product was eluted with methanol/NH3 yielding 9.8 mg (93.4%) of the title compound

Sources & evidence

ORD record
ord-d40c6d79e37d447da0f54dcf6d889d61
Source dataset
uspto-grants-2015_03
Patent number
US08987273B2

Reaction notes

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