Potassium Carbonate → HCID 88426431, compound

HRID 465988Notes

Reaction equation

HRID 465988 reaction equation
[N:1]1[CH:6]=[CH:5][CH:4]=[C:3]([C:7]([C:9]2[CH:14]=[CH:13][CH:12]=[C:11]([NH:15][S:16]([C:19]3[CH:24]=[CH:23][C:22]([Cl:25])=[CH:21][CH:20]=3)(=[O:18])=[O:17])[CH:10]=2)=O)[CH:2]=1.[Cl-].[OH:27][NH3+:28].C(=O)([O-])[O-].[K+].[K+]>C(O)C>[N:1]1[CH:6]=[CH:5][CH:4]=[C:3]([C:7](=[N:28][OH:27])[C:9]2[CH:14]=[CH:13][CH:12]=[C:11]([NH:15][S:16]([C:19]3[CH:24]=[CH:23][C:22]([Cl:25])=[CH:21][CH:20]=3)(=[O:18])=[O:17])[CH:10]=2)[CH:2]=1

Participants

5

Reactant 3

HCID 11430Potassium CarbonateHCID 21645Hydroxylamine HClHCID 149893984-Chloro-N-[3-(pyridine-3-carbonyl)phenyl]benzene-1-sulfonamide

Product 1

HCID 88426431HCID 88426431, compound

Reagents, catalysts & solvents 1

HCID 702EthanolSolvent

Procedure

7.45 g (20 mmol) of the compound from Example 1, 2.08 g (30 mmol) of hydoxylammonium chloride and 4.14 g (30 mmol) of potassium carbonate are refluxed in 20 ml of ethanol for 15 h. After cooling to room temperature, the mixture is evaporated and the residue is stirred in 50 ml of water for 3 h (after this time no oily residues, but only crystalline residues, were still undissolved). The precipitate was filtered off, washed with water and recrystallised from methanol by addition of water. Yield: 5.71 g (73.7% of theory) M.p.: 170° C.

Workup

  1. customthe mixture is evaporated
  2. filtrationThe precipitate was filtered off
  3. washwashed with water
  4. customrecrystallised from methanol by addition of water

Sources & evidence

ORD record
ord-718d871338834745b711958b6d497b62
Source dataset
uspto-grants-1992_10
Patent number
US05155121

Reaction notes

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