Sodium Bicarbonate → HCID 60123143, compound

HRID 2415698Notes

Reaction equation

HRID 2415698 reaction equation
[CH3:1][O:2][C:3]([CH:5]1[CH2:10][CH2:9][CH2:8][N:7]2[C:11](=[O:29])[C:12]([C:22]3[CH:27]=[CH:26][C:25]([F:28])=[CH:24][CH:23]=3)=[C:13]([C:14]3[CH:19]=[CH:18][N:17]=[C:16](SC)[N:15]=3)[N:6]12)=[O:4].[CH2:30]1COCC1.CO.O[O:38][S:39]([O-:41])=O.[K+].C([O-])(O)=O.[Na+]>O.[Cl-].[Na+].O.C(OCC)(=O)C>[CH3:1][O:2][C:3]([C@@H:5]1[CH2:10][CH2:9][CH2:8][N:7]2[C:11](=[O:29])[C:12]([C:22]3[CH:23]=[CH:24][C:25]([F:28])=[CH:26][CH:27]=3)=[C:13]([C:14]3[CH:19]=[CH:18][N:17]=[C:16]([S:39]([CH3:30])(=[O:41])=[O:38])[N:15]=3)[N:6]12)=[O:4]

Participants

8

Reactant 4

HCID 516892Sodium BicarbonateHCID 21899815MeOH tetrahydrofuranHCID 23526874HCID 23526874, compoundHCID 23707502Potassium hydroxy sulfite

Product 1

HCID 60123143HCID 60123143, compound

Reagents, catalysts & solvents 3

HCID 962WaterSolventHCID 8857Ethyl AcetateSolventHCID 57417360Sodium chloride; waterSolvent

Procedure

To a solution of 2-(4-fluorophenyl)-3-(2-methylsulfanylpyrimidin-4-yl)-1-oxo-5,6,7,8-tetrahydro-1H -pyrazolo[1,2-a]pyridazine-5-carboxylic acid methyl ester, 31, (0.48 g, 1.16 mmol) 1:1 THF/methanol (50 mL) is added Oxone® (2.14 g, 3.5 mmol) in water (50 mL). The reaction mixture is stirred for 5 hours at room temperature, reduced in volume in vacuo to about 25 mL and ethyl acetate (200 mL) is added. The organic phase is treated with NaHCO3, brine, dried, and concentrated in vacuo to afford 0.5 g of the desired product as a yellow solid.

Workup

  1. additionis added
  2. customdried
  3. concentrationconcentrated in vacuo

Sources & evidence

ORD record
ord-0c0e6d8f28c9423994df3d5c421737a6
Source dataset
uspto-grants-2004_11
Patent number
US06821971B2

Reaction notes

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