Hydrogen chloride-ethyl acetate → HCID 66697776, compound

HRID 340603Notes

Reaction equation

HRID 340603 reaction equation
C(O[C:6](=O)[N:7]([CH2:9][C:10]1[CH:14]=[C:13]([S:15]([C:18]2[CH:23]=[CH:22][C:21]([F:24])=[CH:20][CH:19]=2)(=[O:17])=[O:16])[N:12]([C:25]2[C:26]([F:31])=[N:27][CH:28]=[CH:29][CH:30]=2)[N:11]=1)C)(C)(C)C.C(OCC)(=O)C.[ClH:39]>C(OCC)(=O)C.CC(O)C>[ClH:39].[F:24][C:21]1[CH:22]=[CH:23][C:18]([S:15]([C:13]2[N:12]([C:25]3[C:26]([F:31])=[N:27][CH:28]=[CH:29][CH:30]=3)[N:11]=[C:10]([CH2:9][NH:7][CH3:6])[CH:14]=2)(=[O:16])=[O:17])=[CH:19][CH:20]=1

Participants

5

Reactant 2

HCID 21866389Hydrogen chloride-ethyl acetateHCID 66697787HCID 66697787, compound

Product 1

HCID 66697776HCID 66697776, compoundYield 73%

Reagents, catalysts & solvents 2

HCID 3776IsopropanolSolventHCID 8857Ethyl AcetateSolvent

Procedure

tert-Butyl({5-[(4-fluorophenyl)sulfonyl]-1-(2-fluoropyridin-3-yl)-1H-pyrazol-3-yl}methyl)methylcarbamate (132 mg) was dissolved in ethyl acetate (2 ml) and 2-propanol (1 mL), and 4 mol/L hydrogen chloride-ethyl acetate solution (3 mL) was added. After stirring at room temperature for 2 hr, the reaction mixture was concentrated under reduced pressure, and the residue was recrystallized from a mixed solvent of ethanol and ethyl acetate to give the title compound as colorless crystals (yield 83 mg, yield 73%). melting point 211-214° C.

Workup

  1. concentrationthe reaction mixture was concentrated under reduced pressure
  2. customthe residue was recrystallized from a mixed solvent of ethanol and ethyl acetate

Sources & evidence

ORD record
ord-00e0254d7cb540eb9ecc7f17f2262b9b
Source dataset
uspto-grants-2014_11
Patent number
US08895588B2

Reaction notes

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