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Methanol → methyl 2-[(4,6-dimethoxytriazin-2-y1)oxy]-6-[1-(N-methoxyimino)ethyl]benzoate

HRID 4908
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 4908
[C:1]([C:4]1[CH:13]=[CH:12][CH:11]=[C:10]([O:14][N:15]2[N:20]=[C:19]([O:21][CH3:22])[CH:18]=[C:17]([O:23][CH3:24])[NH:16]2)[C:5]=1[C:6]([O:8][CH3:9])=[O:7])(=O)[CH3:2].Cl.[CH3:26][O:27][NH2:28].C([O-])(=O)C.[K+].CO>O>[CH3:22][O:21][C:19]1[CH:18]=[C:17]([O:23][CH3:24])[NH:16][N:15]([O:14][C:10]2[CH:11]=[CH:12][CH:13]=[C:4]([C:1](=[N:28][O:27][CH3:26])[CH3:2])[C:5]=2[C:6]([O:8][CH3:9])=[O:7])[N:20]=1
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Komponenten

6

Edukt 4

HCID 887MethanolHCID 517044Potassium AcetateHCID 521874O-Methylhydroxylamine hydrochlorideHCID 19089388Methyl 2-acetyl-6-[(4,6-dimethoxytriazin-2-yl)oxy]benzoate

Produkt 1

HCID 86747186methyl 2-[(4,6-dimethoxytriazin-2-y1)oxy]-6-[1-(N-methoxyimino)ethyl]benzoateAusbeute 48 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 962WaterLösungsmittel

Versuchsvorschrift

0.9 of methyl 2-acetyl-6-[(4,6-dimethoxytriazin-2-yl)oxy]benzoate, 0.68 g of methoxyamine hydrochloride and 0.80 g of potassium acetate were added to 30 ml of methanol, and the resultant mixture was stirred for one day and one night at room temperature. The resultant reaction liquor was poured into water, and was extracted with ethyl acetate. After washing the extracted product with water, the washed product was dried and concentrated to obtain an oily product. This was then purified by column chromatography to obtain 0.47 g of the aimed compound (melting point=131° to 135° C.) at a yield of 48%.

Aufarbeitung

  1. customThe resultant reaction liquor
  2. extractionwas extracted with ethyl acetate
  3. washAfter washing the extracted product with water
  4. customthe washed product was dried
  5. concentrationconcentrated
  6. customto obtain an oily product
  7. customThis was then purified by column chromatography

Quellen und Nachweise

ORD-Eintrag
ord-9caf7f2af9b04e69903afed00c9e43d0
Quelldatensatz
uspto-grants-1993_09
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US05242895

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