Sodium Carbonate → HCID 9801486, compound

HRID 1270154Notes

Reaction equation

HRID 1270154 reaction equation
[NH2:1][CH2:2][CH2:3][NH:4][C:5]1[C:6]2[N:7]([C:16](=[O:19])[NH:17][N:18]=2)[C:8]2[C:13]([N:14]=1)=[CH:12][CH:11]=[C:10]([F:15])[CH:9]=2.Cl[C:21]1[CH:26]=[CH:25][C:24]([C:27]([F:30])([F:29])[F:28])=[CH:23][N:22]=1.C(=O)([O-])[O-].[Na+].[Na+]>C(O)CCC>[F:15][C:10]1[CH:9]=[C:8]2[C:13]([N:14]=[C:5]([NH:4][CH2:3][CH2:2][NH:1][C:21]3[CH:26]=[CH:25][C:24]([C:27]([F:30])([F:29])[F:28])=[CH:23][N:22]=3)[C:6]3[N:7]2[C:16](=[O:19])[NH:17][N:18]=3)=[CH:12][CH:11]=1

Participants

5

Reactant 3

HCID 10340Sodium CarbonateHCID 923422-Chloro-5-(trifluoromethyl)pyridineHCID 18449173HCID 18449173, compound

Product 1

HCID 9801486HCID 9801486, compound

Reagents, catalysts & solvents 1

HCID 2631-ButanolSolvent

Procedure

A solution of 259 mg of 4-(2-amino-ethylamino)-8-fluoro-2H-[1,2,4]triazolo[4,3-a]quinoxalin-1-one, 422 mg of 2-chloro-5-trifluoromethylpyridine and 411 mg of sodium carbonate in n-butanol (1 mL) was heated to reflux for 48 hrs. The reaction mixture was cooled to room temperature, filtered through diatomaceous earth, and the filtrate concentrated to give a solid residue. This was separated by silica gel chromatography to provide the title compound. MS (M+H)+=407.9.

Workup

  1. temperatureto reflux for 48 hrs
  2. filtrationfiltered through diatomaceous earth
  3. concentrationthe filtrate concentrated
  4. customto give a solid residue
  5. customThis was separated by silica gel chromatography

Sources & evidence

ORD record
ord-265f5e1acb3945ffbf4e1bea8e56a308
Source dataset
uspto-grants-2007_04
Patent number
US07202245B2

Reaction notes

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