O-Methylhydroxylamine hydrochloride → 4-bromo-N-(methoxyiminomethyl)-2-methyl benzoic acid amide

HRID 1187994Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1187994
[Br:1][C:2]1[CH:14]=[CH:13][C:5]([C:6]([N:8]=[CH:9][N:10](C)C)=[O:7])=[C:4]([CH3:15])[CH:3]=1.Cl.[CH3:17][O:18]N>O1CCOCC1.O.C(OCC)(=O)C>[Br:1][C:2]1[CH:14]=[CH:13][C:5]([C:6]([NH:8][CH:9]=[N:10][O:18][CH3:17])=[O:7])=[C:4]([CH3:15])[CH:3]=1

Komponenten

6

Edukt 2

HCID 521874O-Methylhydroxylamine hydrochlorideHCID 666997874-Bromo-N-[(dimethylamino)methylene]-2-methylbenzamide

Produkt 1

HCID 1363378164-bromo-N-(methoxyiminomethyl)-2-methyl benzoic acid amideAusbeute 103,7 %

Reagenzien, Katalysatoren, Lösungsmittel 3

HCID 962WaterLösungsmittelHCID 8857Ethyl AcetateLösungsmittelHCID 312751,4-DioxaneLösungsmittel

Versuchsvorschrift

In a solution of 0.67 g of 4-bromo-N-(dimethylaminomethylidene)-2-methyl benzoic acid amide in 10 mL of 1,4-dioxane, a solution of 0.36 g of methoxyamine hydrochloride in 2 mL of water was added, and stirred at room temperature for 1 hour. After the completion of the reaction, the reaction mixture was diluted with 50 mL of ethyl acetate, washed with water, and dehydrated with and dried over saturated sodium chloride aqueous solution and then anhydrous magnesium sulfate, and the solvent was distilled off under reduced pressure to obtain 0.70 g of the aimed product as white crystal.

Aufarbeitung

  1. customAfter the completion of the reaction
  2. washwashed with water
  3. dry with materialdried over saturated sodium chloride aqueous solution
  4. distillationanhydrous magnesium sulfate, and the solvent was distilled off under reduced pressure

Quellen und Nachweise

ORD-Eintrag
ord-7306445de2b8419397711a611fa5194a
Quelldatensatz
uspto-grants-2014_03
Patentnummer
US08673951B2

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