Water → HCID 13629660, Verbindung

HRID 255493Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 255493
C[NH:2][O:3]C.C([N:7]([CH2:10]C)CC)C.[Cl:12][C:13]1[CH:29]=[C:28]([C:30]([F:33])([F:32])[F:31])[CH:27]=[CH:26][C:14]=1[O:15][C:16]1[CH:17]=[C:18]([CH2:22][C:23](Cl)=[O:24])[CH:19]=[CH:20][CH:21]=1.[OH2:34].CN(C)[C:37](=[O:39])C>>[CH3:10][N:7]([O:39][CH3:37])[C:23](=[O:24])[CH2:22][C:18]1[CH:17]=[C:16]([O:15][C:14]2[CH:26]=[CH:27][C:28]([C:30]([F:33])([F:32])[F:31])=[CH:29][C:13]=2[Cl:12])[CH:21]=[CH:20][C:19]=1[N+:2]([O-:3])=[O:34]

Komponenten

6

Edukt 5

HCID 962WaterHCID 8471TriethylamineHCID 14232N,O-DimethylhydroxylamineHCID 31374DimethylacetamideHCID 13630154{3-[2-Chloro-4-(trifluoromethyl)phenoxy]phenyl}acetyl chloride

Produkt 1

HCID 13629660HCID 13629660, Verbindung

Versuchsvorschrift

0.9 g of N,O-dimethylhydroxylamine and 1.5 g of triethylamine were dissolved in 20 ml of N,N-dimethylacetamide at 5° C., followed by addition of 3.5 g of 3-(2'-chloro-4'-trifluoromethylphenoxy)phenylacetyl chloride. The reaction was allowed to proceed at 5° C. for 1 hour and then at room temperature for further 3 hours to complete the reaction. After completion of the reaction, 50 ml of water was added to the liquid reaction mixture, followed by extraction twice with 30 ml portions of ether. The ether layer was washed with dilute hydrochloric acid and water and dried over anhydrous sodium sulfate, and the ether was distilled off under reduced pressure to obtain 3.5 g of N-methyl-N-methoxy-2-nitro-5-(2'-chloro-4'-trifluoromethylphenoxy)phenylacetamide.

Aufarbeitung

  1. waitat room temperature for further 3 hours to complete
  2. customthe reaction
  3. additionwas added to the liquid reaction mixture
  4. extractionfollowed by extraction twice with 30 ml portions of ether
  5. washThe ether layer was washed with dilute hydrochloric acid and water
  6. dry with materialdried over anhydrous sodium sulfate
  7. distillationthe ether was distilled off under reduced pressure

Quellen und Nachweise

ORD-Eintrag
ord-9e363918f8204b4f89976ead429501ce
Quelldatensatz
uspto-grants-1987_10
Patentnummer
US04698094

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