Succinic Acid → HCID 131729280, compound

HRID 557290Notes

Reaction equation

HRID 557290 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]([OH:35])(=[O:34])[CH2:29][CH2:30][C:31]([OH:33])=[O:32]>CO>[C:28]([OH:35])(=[O:34])[CH2:29][CH2:30][C:31]([OH:33])=[O:32].[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.[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 1110Succinic AcidHCID 16719049E-1210

Product 1

HCID 131729280HCID 131729280, compoundYield 35.6%

Reagents, catalysts & solvents 1

HCID 887MethanolSolvent

Procedure

3-(3-(4-(Pyridin-2-yloxymethyl)-benzyl)-isoxazol-5-yl)-pyridin-2-yl amine (200 mg) was dissolved in methanol (10 mL), and succinic acid (65.8 mg) was added thereto. This reaction mixture as stirred at room temperature for 5 minutes, and then, concentrated under a reduced pressure. To the residue was added ethanol (10 mL), heated using an oil bath at 60° C, then cooled to 0° C to cause a solid to be precipitated. The solids were collected, washed with ethanol, and then, dried in vacuo to obtain the title compound (83 mg).

Workup

  1. concentrationconcentrated under a reduced pressure
  2. additionTo the residue was added ethanol (10 mL)
  3. temperatureheated
  4. customat 60° C
  5. temperaturecooled to 0° C
  6. customto be precipitated
  7. customThe solids were collected
  8. washwashed with ethanol
  9. customdried in vacuo

Sources & evidence

ORD record
ord-e4a34d4df9d0419ea02474c344e40591
Source dataset
uspto-grants-2011_11
Patent number
US08058444B2

Reaction notes

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