Benzenesulfonic Acid → HCID 25070765, compound

HRID 557286Notes

Reaction equation

HRID 557286 reaction equation
[N:1]1[CH:6]=[CH:5][CH:4]=[CH:3][C:2]=1[O:7][CH2:8][C:9]1[CH:27]=[CH:26][C:12]([CH2:13][C:14]2[CH:18]=[C:17]([C:19]3[C:20]([NH2:25])=[N:21][CH:22]=[CH:23][CH:24]=3)[O:16][N:15]=2)=[CH:11][CH:10]=1.[C:28]1([S:34]([OH:37])(=[O:36])=[O:35])[CH:33]=[CH:32][CH:31]=[CH:30][CH:29]=1>CO>[C:28]1([S:34]([OH:37])(=[O:36])=[O:35])[CH:33]=[CH:32][CH:31]=[CH:30][CH:29]=1.[N:1]1[CH:6]=[CH:5][CH:4]=[CH:3][C:2]=1[O:7][CH2:8][C:9]1[CH:27]=[CH:26][C:12]([CH2:13][C:14]2[CH:18]=[C:17]([C:19]3[C:20]([NH2:25])=[N:21][CH:22]=[CH:23][CH:24]=3)[O:16][N:15]=2)=[CH:11][CH:10]=1

Participants

4

Reactant 2

HCID 7371Benzenesulfonic AcidHCID 16719049E-1210

Product 1

HCID 25070765HCID 25070765, compoundYield 74.2%

Reagents, catalysts & solvents 1

HCID 887MethanolSolvent

Procedure

3-(3-(4-(Pyridin-2-yloxymethyl)-benzyl)-isoxazol-5-yl)-pyridin-2-yl amine (100 mg) was dissolved in methanol (5 mL) and benzenesulfonic acid (46.3 mg) was added thereto. This solution was stirred at room temperature for 5 minutes, and then, concentrated in vacuo. To the residue was added ethanol (5 mL), and subjected to ultrasound treatment to cause solids to be precipitated. This solids were filtered, washed with ethanol, and then, dried under a reduced pressure to obtain the title compound (107 mg).

Workup

  1. concentrationconcentrated in vacuo
  2. additionTo the residue was added ethanol (5 mL)
  3. customto be precipitated
  4. filtrationThis solids were filtered
  5. washwashed with ethanol
  6. customdried under a reduced pressure

Sources & evidence

ORD record
ord-5c3681626db4456bac099d16c6ff1f41
Source dataset
uspto-grants-2011_11
Patent number
US08058444B2

Reaction notes

Loading…