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Hydrochloric Acid → HCID 21226466, compound

HRID 583042
Notes
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Reaction equation

HRID 583042 reaction equation
[OH-].[Na+].C([O:6][CH2:7][C:8]1[CH:9]=[C:10]([C:15]2[C:19]([Cl:20])=[C:18]([O:21][CH:22]([F:24])[F:23])[N:17]([CH3:25])[N:16]=2)[CH:11]=[CH:12][C:13]=1[Cl:14])(=O)C.Cl>O1CCOCC1.O>[Cl:20][C:19]1[C:15]([C:10]2[CH:11]=[CH:12][C:13]([Cl:14])=[C:8]([CH2:7][OH:6])[CH:9]=2)=[N:16][N:17]([CH3:25])[C:18]=1[O:21][CH:22]([F:24])[F:23]
ParticipantsProcedureWorkupSources & evidenceReaction notes

Participants

6

Reactant 3

HCID 313Hydrochloric AcidHCID 14798Sodium HydroxideHCID 21226441HCID 21226441, compound

Product 1

HCID 21226466HCID 21226466, compound

Reagents, catalysts & solvents 2

HCID 962WaterSolventHCID 312751,4-DioxaneSolvent

Procedure

6.3 ml (16 mmol) of 10% strength sodium hydroxide solution were added dropwise to a solution of 3.2 g (8.8 mmol) of 3-(3-acetoxymethyl-4-chlorophenyl)-4-chloro-5-difluoromethoxy-1-methyl-1H-pyrazole in 10 ml of dioxane and 10 ml of water. The mixture was stirred for 1 hour and then neutralized with 3N hydrochloric acid. The product was extracted from the aqueous phase with ethyl acetate, after which the organic phase was dried over magnesium sulfate and then concentrated. The crude product thus obtained was purified by column chromography on silica gel (eluent: hexane/ethyl acetate=4:1). Yield: 1.3 g.

Workup

  1. extractionThe product was extracted from the aqueous phase with ethyl acetate
  2. dry with materialafter which the organic phase was dried over magnesium sulfate
  3. concentrationconcentrated

Sources & evidence

ORD record
ord-aee0fdb0511c472e9c91ae8c7cb2c2d6
Source dataset
uspto-grants-1999_07
DOI
10.6084/m9.figshare.5104873.v1
Patent number
US05928999

Reaction notes

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On this pageParticipantsProcedureWorkupSources & evidenceReaction notes