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Acetone, oxime → 5-Acetyl-2-(2-chlorophenylamino)-3-fluoro-4-isopropylideneaminooxybenzoic acid methyl ester

HRID 1788231
Notes
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Reaction equation

HRID 1788231 reaction equation
CC([O-])(C)C.[K+].[CH3:7][C:8](=[N:10][OH:11])[CH3:9].[CH3:12][O:13][C:14](=[O:34])[C:15]1[CH:20]=[C:19]([C:21](=[O:23])[CH3:22])[C:18](F)=[C:17]([F:25])[C:16]=1[NH:26][C:27]1[CH:32]=[CH:31][CH:30]=[CH:29][C:28]=1[Cl:33]>C1COCC1>[CH3:12][O:13][C:14](=[O:34])[C:15]1[CH:20]=[C:19]([C:21](=[O:23])[CH3:22])[C:18]([O:11][N:10]=[C:8]([CH3:9])[CH3:7])=[C:17]([F:25])[C:16]=1[NH:26][C:27]1[CH:32]=[CH:31][CH:30]=[CH:29][C:28]=1[Cl:33]
ParticipantsConditionsProcedureWorkupSources & evidenceReaction notes

Participants

5

Reactant 3

HCID 67180Acetone, oximeHCID 23665647Potassium tert-butoxideHCID 865967735-Acetyl-2-(2-chlorophenylamino)-3,4-difluorobenzoic acid methyl ester

Product 1

HCID 865967745-Acetyl-2-(2-chlorophenylamino)-3-fluoro-4-isopropylideneaminooxybenzoic acid methyl ester

Reagents, catalysts & solvents 1

HCID 8028Tetrahydrofuran
Solvent
2×

Conditions

Temperature
-78 °C

Procedure

t-BuOK (0.47 mL, 1.0 M in THF) was added to propan-2-one oxime (35 mg, 0.47 mmol). After stirring for 30 minutes, THF (0.5 mL) was added, and the reaction mixture was cooled to −78° C. A solution of 5-acetyl-2-(2-chlorophenylamino)-3,4-difluorobenzoic acid methyl ester (6) (50.0 mg, 0.147 mmol) in THF (1 mL) was added. The reaction mixture was slowly warmed to 0° C. and stirred for 2 hours. The reaction mixture was quenched with saturated aqueous NH4Cl, diluted with EtOAc and water. The aqueous layer was separated and extracted with EtOAc. The combined organic extracts were dried over MgSO4, filtered, and concentrated in vacuo to give the 5-acetyl-2-(2-chloro-phenylamino)-3-fluoro-4-isopropylideneaminooxy-benzoic acid methyl ester. The recovered oxime was suspended in a 1:1 mixture of 5% aqueous HCl and MeOH (30 ml) and heated to reflux. After 1 hour, the reaction mixture was cooled to room temperature and diluted with EtOAc. The organic layer was washed with water, dried (MgSO4) and concentrated. Purification by flash column chromatography using the Biotage system (40% methylene chloride in hexanes) provided 17 mg (35% for two steps) of the desired product (7).

Workup

  1. temperatureThe reaction mixture was slowly warmed to 0° C.
  2. stirringstirred for 2 hours
  3. customThe reaction mixture was quenched with saturated aqueous NH4Cl
  4. additiondiluted with EtOAc and water
  5. customThe aqueous layer was separated
  6. extractionextracted with EtOAc
  7. dry with materialThe combined organic extracts were dried over MgSO4
  8. filtrationfiltered
  9. concentrationconcentrated in vacuo

Sources & evidence

ORD record
ord-7e0c62ff7ef94994b0999cfd90568b5e
Source dataset
uspto-grants-2009_03
DOI
10.6084/m9.figshare.5104873.v1
Patent number
US07511058B2

Reaction notes

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On this pageParticipantsConditionsProcedureWorkupSources & evidenceReaction notes