Hydrochloric Acid → HCID 86650131, compound

HRID 2197497Notes

Reaction equation

HRID 2197497 reaction equation
[F:1][CH:2]([F:35])[O:3][C:4]1[N:8]([CH3:9])[N:7]=[C:6]([C:10]([F:13])([F:12])[F:11])[C:5]=1[C:14]1[C:23](=[O:24])[N:22]([CH2:25][CH:26]([F:28])[F:27])[C:17]2=[N:18][CH:19]=[CH:20][N:21]=[C:16]2[C:15]=1[O:29]C(=O)C(C)C.[OH-].[Na+].Cl>CO.O>[F:35][CH:2]([F:1])[O:3][C:4]1[N:8]([CH3:9])[N:7]=[C:6]([C:10]([F:12])([F:13])[F:11])[C:5]=1[C:14]1[C:23](=[O:24])[N:22]([CH2:25][CH:26]([F:27])[F:28])[C:17]2=[N:18][CH:19]=[CH:20][N:21]=[C:16]2[C:15]=1[OH:29]

Participants

6

Reactant 3

HCID 313Hydrochloric AcidHCID 14798Sodium HydroxideHCID 44129699HCID 44129699, compound

Product 1

HCID 86650131HCID 86650131, compound

Reagents, catalysts & solvents 2

HCID 887MethanolSolventHCID 962WaterSolvent2×

Procedure

A solution of isobutyric acid 7-(5-difluoromethoxy-1-methyl-3-trifluoromethyl-1H-pyrazol-4-yl)-5-(2,2-difluoroethyl)-6-oxo-5,6-dihydro-pyrido[2,3-b]pyrazin-8-yl ester (Example 2.8) (0.138 g), sodium hydroxide (0.022 g) in methanol (4 ml) and water (1 ml) were stirred at ambient temperature for 3 hours. The reaction mixture was poured into water and neutralised by addition of aqueous hydrochloric acid (2M). The mixture was extracted with ethyl acetate. The organic phase was washed with water, aqueous sodium hydrogen carbonate (saturated) and brine, dried over anhydrous sodium sulfate and concentrated to give Compound No. B25 of Table B (0.095 g).

Workup

  1. extractionThe mixture was extracted with ethyl acetate
  2. washThe organic phase was washed with water, aqueous sodium hydrogen carbonate (saturated) and brine
  3. dry with materialdried over anhydrous sodium sulfate
  4. concentrationconcentrated
  5. customto give Compound No

Sources & evidence

ORD record
ord-814ab1b63fa74b5e98567206f0fb63c5
Source dataset
uspto-grants-2012_12
Patent number
US08338598B2

Reaction notes

Loading…