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Hydrochloric Acid → Desmethylamino Methoxy (E)-Metominostrobin

HRID 1769406
Notes
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Reaction equation

HRID 1769406 reaction equation
[CH3:1][O:2]/[N:3]=[C:4](\[C:7]1[CH:12]=[CH:11][CH:10]=[CH:9][C:8]=1[O:13][C:14]1[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=1)/[C:5]#N.Cl.[C:21](=O)(O)[O-:22].[Na+].C[OH:27]>>[CH3:21][O:22][C:5](=[O:27])/[C:4](/[C:7]1[CH:12]=[CH:11][CH:10]=[CH:9][C:8]=1[O:13][C:14]1[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=1)=[N:3]/[O:2][CH3:1]
ParticipantsProcedureWorkupSources & evidenceReaction notes

Participants

5

Reactant 4

HCID 313Hydrochloric AcidHCID 887MethanolHCID 516892Sodium BicarbonateHCID 11128775(1E)-N-methoxy-2-phenoxybenzenecarboximidoyl cyanide

Product 1

HCID 10803045Desmethylamino Methoxy (E)-MetominostrobinYield 46.7%

Procedure

To E-α-methoxyimino-2-phenoxyphenylacetonitrile (a mixture of E- and Z-isomers) (0.76 g, 0.003 mole) was added 30% hydrochloric acid in methanol (4.5 ml) and the mixture was stirred under reflux for 22 hours. After completion of the reaction, 8% aqueous solution of sodium bicarbonate (100 ml) was added to the reaction mixture and extracted with methylene chloride. The extract was dried over anhydrous magnesium sulfate and concentrated under reduced pressure. The resulting residue was purified by silica gel chromatography (ethyl acetate/n-hexane) to obtain E-α-methoxyimino-2-phenoxyphenylacetic acid methyl ester (0.40 g, 46.7%) as colorless crystals (melting point: 109°-110° C.).

Workup

  1. temperatureunder reflux for 22 hours
  2. additionwas added to the reaction mixture
  3. extractionextracted with methylene chloride
  4. dry with materialThe extract was dried over anhydrous magnesium sulfate
  5. concentrationconcentrated under reduced pressure
  6. customThe resulting residue was purified by silica gel chromatography (ethyl acetate/n-hexane)

Sources & evidence

ORD record
ord-44a89ae673204553a37b7844e9e5d377
Source dataset
uspto-grants-1995_01
DOI
10.6084/m9.figshare.5104873.v1
Patent number
US05380913

Reaction notes

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On this pageParticipantsProcedureWorkupSources & evidenceReaction notes