Hydrochloric Acid → HCID 178502623, Verbindung

HRID 612806Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 612806
CC(C)([O-])C.[K+].[CH3:7][O:8][N:9]=[C:10]1[C:14]2[CH:15]=[CH:16][CH:17]=[CH:18][C:13]=2[O:12][CH2:11]1.[N:19](OC(C)(C)C)=[O:20].Cl>C(O)(C)(C)C>[CH3:7][O:8][N:9]=[C:10]1[C:14]2[CH:15]=[CH:16][CH:17]=[CH:18][C:13]=2[O:12][C:11]1=[N:19][OH:20]

Komponenten

6

Edukt 4

HCID 313Hydrochloric AcidHCID 10906Tert-Butyl nitriteHCID 23665647Potassium tert-butoxideHCID 54271616benzofuran-3-one O-methyl oxime

Produkt 1

HCID 178502623HCID 178502623, VerbindungAusbeute 47,4 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6386tert-ButanolLösungsmittel2×

Versuchsvorschrift

3.92 g (0.035 mol) of potassium tert-butoxide are dissolved in 40 ml of tert-butanol. A solution of 5.7 g (0.035 mol) of benzofuran-3-one O-methyl-oxime and 7.2 g (0.07 mol) of tert-butyl nitrite in 10 ml of tert-butanol is added to this solution. The mixture is stirred without cooling for two hours and then admixed with 20 ml of 2N aqueous hydrochloric acid. The crystalline product is filtered off, washed repeatedly with water and dried in a desiccator. 3.19 g (47.1% of theory) of benzofuran-2,3-dione 3-(O-methyl-oxime) 2-oxime are obtained as a mixture of two stereoisomers comprising 86.33% of isomer A and 12.98% of isomer B (HPLC).

Aufarbeitung

  1. temperaturewithout cooling for two hours
  2. filtrationThe crystalline product is filtered off
  3. washwashed repeatedly with water
  4. customdried in a desiccator

Quellen und Nachweise

ORD-Eintrag
ord-c8902eb2e08d49ddacccd338e7b6ef37
Quelldatensatz
uspto-grants-1999_12
Patentnummer
US06005104

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