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Ethanol → 2,6-Dichloro-3-nitrobenzylideneaminooxyacetic Acid

HRID 905367
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 905367
Cl[C:2]1[C:9]([N+:10]([O-:12])=[O:11])=[CH:8][CH:7]=[C:6]([Cl:13])[C:3]=1[CH:4]=O.C(O)C.[ClH:17].[C:18]([CH2:21][O:22][NH2:23])([OH:20])=[O:19].C(CON)(O)=O.C([O-])(=O)C.[Na+]>O>[Cl:17][CH:21]([O:22][N:23]=[CH:4][C:3]1[C:6]([Cl:13])=[CH:7][CH:8]=[C:9]([N+:10]([O-:12])=[O:11])[CH:2]=1)[C:18]([OH:20])=[O:19]
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

6

Edukt 4

HCID 702EthanolHCID 517045Sodium AcetateHCID 2723609Aminooxyacetic acid hemihydrochlorideHCID 27949122,6-Dichloro-3-nitrobenzaldehyde

Produkt 1

HCID 1317133262,6-Dichloro-3-nitrobenzylideneaminooxyacetic Acid

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 962
Water
Lösungsmittel

Versuchsvorschrift

A warm solution of 2,6-dichloro-3-nitrobenzaldehyde, 1.8 gm. in 20 ml. of ethanol was stirred into a solution of 0.9 gm. (0.008 equivs.) of carboxymethoxylamine hemihydrochloride and 0.45 gm. of sodium acetate, anhyd., in 20 ml. of water at room temperature. The mixture was heated on the steam bath for one-half hour, and was then evaporated to dryness at room temperature. The residue was triturated with cold water, filtered, washed with cold water and dried in air to obtain 2.1 gm. (87.4%) of crude material melting at 76°-84° C. This was purified from aqueous-methanol to obtain 1.9 gm. of pale cream-colored product melting at 82°-85° C.

Aufarbeitung

  1. customat room temperature
  2. temperatureThe mixture was heated on the steam bath for one-half hour
  3. customwas then evaporated to dryness at room temperature
  4. customThe residue was triturated with cold water
  5. filtrationfiltered
  6. washwashed with cold water
  7. customdried in air
  8. customto obtain 2.1 gm
  9. customThis was purified from aqueous-methanol
  10. customto obtain 1.9 gm

Quellen und Nachweise

ORD-Eintrag
ord-53d2f437ebe943f9bff6bf863ea181a4
Quelldatensatz
uspto-grants-1983_12
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US04423241

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