Hydrochloride methanol → HCID 178432457, compound

HRID 1991449Notes

Reaction equation

HRID 1991449 reaction equation
[OH:1][C:2]1[N:6]([C:7]2[CH:12]=[CH:11][CH:10]=[CH:9][CH:8]=2)[N:5]=[C:4]([CH3:13])[C:3]=1[CH:14]1[C:22]2[C:21]([OH:23])=[C:20]([CH3:24])[N:19]=[CH:18][C:17]=2[CH2:16][O:15]1.[ClH:25].CO>CO>[ClH:25].[OH:1][C:2]1[N:6]([C:7]2[CH:8]=[CH:9][CH:10]=[CH:11][CH:12]=2)[N:5]=[C:4]([CH3:13])[C:3]=1[CH:14]1[C:22]2[C:21]([OH:23])=[C:20]([CH3:24])[N:19]=[CH:18][C:17]=2[CH2:16][O:15]1

Participants

4

Reactant 2

HCID 21893726Hydrochloride methanolHCID 178432456HCID 178432456, compound

Product 1

HCID 178432457HCID 178432457, compoundYield 90%

Reagents, catalysts & solvents 1

HCID 887MethanolSolvent

Conditions

Temperature
4 °C

Procedure

0.5006 g of 1-(5-hydroxy-3-methyl-1-phenyl-1-H-pyrazol-4-yl)-6-methyl-1,3-dihydro-furo[3,4-c]pyridin-7-ol was solved in 150 mL of methanol, and 2N of methanol hydrochloride (1.65 mL) was added and stirred. The solution was concentrated to about 20 mL, and when crystals were precipitate, 50 mL of ethanol was added and concentrated to substitute the crystal solvent, and continued this operation twice and concentrated to about 5 mL. This concentrated solution was stood to cool in refrigerator (4° C.) overnight, the precipitate was filtered off and dried in vacuum desiccator to give 1-(5-hydroxy-3-methyl-1-phenyl-1-H-pyrazol-4-yl)-6-methyl-1,3-dihydro-furo[3,4-c]pyridin-7-ol hydrochloride (0.5011 g). Yield 90.0%. Appearance: crystal powder, pale yellow white. Melting point: 247-249° C. (browning melt).

Workup

  1. concentrationThe solution was concentrated to about 20 mL, and when crystals
  2. addition50 mL of ethanol was added
  3. concentrationconcentrated
  4. concentrationconcentrated to about 5 mL
  5. filtrationthe precipitate was filtered off
  6. customdried in vacuum desiccator

Sources & evidence

ORD record
ord-bd8585b1b84e44ba95013febb417e947
Source dataset
uspto-grants-2010_01
Patent number
US07645882B2

Reaction notes

Loading…