Hydrochloric Acid → HCID 66992495, compound

HRID 557277Notes

Reaction equation

HRID 557277 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.[ClH:28]>CO>[ClH:28].[ClH:28].[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 313Hydrochloric AcidHCID 16719049E-1210

Product 1

HCID 66992495HCID 66992495, compound

Reagents, catalysts & solvents 1

HCID 887MethanolSolvent

Procedure

3-(3-(4-(Pyridin-2-yloxymethyl)-benzyl)-isoxazol-5-yl)-pyridin-2-yl amine (1 g) was dissolved in methanol (50 mL), and concentrated hydrochloric acid (1.18 mL) was added thereto at room temperature. This mixed solution was stirred at room temperature for 5 minutes, and then concentrated under a reduced pressure. To the residue were added ethanol and tert-butyl methyl ether, and subjected to ultrasound treatment. The precipitated solids were filtered, washed with tert-butyl methyl ether and dried in vacuo to obtain the title compound (908 mg).

Workup

  1. customat room temperature
  2. concentrationconcentrated under a reduced pressure
  3. additionTo the residue were added ethanol and tert-butyl methyl ether
  4. filtrationThe precipitated solids were filtered
  5. washwashed with tert-butyl methyl ether
  6. customdried in vacuo

Sources & evidence

ORD record
ord-da4db9df84f04e099948624f99699763
Source dataset
uspto-grants-2011_11
Patent number
US08058444B2

Reaction notes

Loading…