Phosphoric Acid → HCID 25070761, compound

HRID 557280Notes

Reaction equation

HRID 557280 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.[P:28](=[O:32])([OH:31])([OH:30])[OH:29]>CO.C(OCC)(=O)C>[P:28]([OH:32])([OH:31])([OH:30])=[O:29].[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

5

Reactant 2

HCID 1004Phosphoric AcidHCID 16719049E-1210

Product 1

HCID 25070761HCID 25070761, compound

Reagents, catalysts & solvents 2

HCID 887MethanolSolventHCID 8857Ethyl AcetateSolvent

Procedure

3-(3-(4-(Pyridin-2-yloxymethyl)-benzyl)-isoxazol-5-yl)-pyridin-2-yl amine (65 mg) was dissolved in methanol (0.87 mL) and ethyl acetate (0.87 mL), and phosphoric acid (85%, 0.013 mL) was added thereto. The solvent was concentrated under a reduced pressure, to the residue was added ethanol (4.3 mL), and dissolved by heating. Then, after filtration, the solution was left at room temperature to be solidified. The solids were filtered to obtain the title compound (31 mg).

Workup

  1. concentrationThe solvent was concentrated under a reduced pressure, to the residue
  2. additionwas added ethanol (4.3 mL)
  3. dissolutiondissolved
  4. temperatureby heating
  5. filtrationThen, after filtration
  6. waitthe solution was left at room temperature
  7. filtrationThe solids were filtered

Sources & evidence

ORD record
ord-b66c588412c94f58899e25a6640e0c20
Source dataset
uspto-grants-2011_11
Patent number
US08058444B2

Reaction notes

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