StartseiteMCPWorkbenchSkills
StartseiteWorkbenchBenachrichtigungenMein Bereich
llms.txt · MCP-AnleitungDatenschutz · Nutzungsbedingungen · Supportv1.8.0
  1. Startseite
  2. /Reaktion

2-Methoxypropene → (Z)-2-(4,5-difluoro-2-hydroxybenzoyl)-3-hydroxypyridine O-t-butyloxime

HRID 862093
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 862093
Br[C:2]1[CH:7]=[C:6]([F:8])[C:5]([F:9])=[CH:4][C:3]=1[OH:10].C[O:12][C:13]([CH3:15])=[CH2:14].[CH3:16]CCCCC.[CH2:22]([Li])CCC.[C:27]([C:29]1[C:34]([O:35][Si](C)(C)C)=[CH:33][CH:32]=[CH:31][N:30]=1)#[N:28]>C(OCC)C>[C:13]([O:12]/[N:28]=[C:27](\[C:29]1[C:34]([OH:35])=[CH:33][CH:32]=[CH:31][N:30]=1)/[C:2]1[CH:7]=[C:6]([F:8])[C:5]([F:9])=[CH:4][C:3]=1[OH:10])([CH3:15])([CH3:16])[CH3:14].[C:13]([O:12]/[N:28]=[C:27](/[C:29]1[C:34]([OH:35])=[CH:33][CH:32]=[CH:31][N:30]=1)\[C:2]1[CH:7]=[C:6]([F:8])[C:5]([F:9])=[CH:4][C:3]=1[OH:10])([CH3:15])([CH3:22])[CH3:14]
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

7

Edukt 4

HCID 83002-MethoxypropeneHCID 27362882-Bromo-4,5-difluorophenolHCID 158191802-Cyano-3-trimethylsilyloxypyridineHCID 178418244HCID 178418244, Verbindung

Produkt 2

HCID 136395970(Z)-2-(4,5-difluoro-2-hydroxybenzoyl)-3-hydroxypyridine O-t-butyloxime
HCID 136395971
(E)-2-(4,5-difluoro-2-hydroxybenzoyl)-3-hydroxypyridine O-t-butyloxime

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 3283Diethyl EtherLösungsmittel

Versuchsvorschrift

A mixture of 2-bromo-4,5-difluorophenol (7.27 g) and 2-methoxypropene (10 ml) was stirred for one hour at room temperature, followed by adding diethyl ether (75 ml) and cooling to -78° C. To the mixture was added dropwise, under argon atmosphere, a 1.6M solution of n-butyl lithium hexane solution (25 ml), followed by stirring for one hour. To the reaction mixture was then added dropwise 2-cyano-3-trimethylsilyloxypyridine (7.01 g). The cooling bath was removed, and the mixture was stirred for 3 hours while warming up to room temperature. To the reaction mixture was added ethanol (10 ml) to quench the reaction. The solvent was distilled off under reduced pressure. To the residue were added triethylamine (20 ml), O-t-butylhydroxylamine hydrochloride (3.06 g) and ethanol (50 ml). The mixture was heated for 5 hours under reflux. The solvent was distilled off. To the residue were added chloroform and water for extraction. The organic layer was dried (anhydrous magnesium sulfate), and the solvent was distilled off under reduced pressure. The residue was purified by means of a silica gel column chromatography (eluted with ethyl acetate/hexane) to give (Z)-2-(4,5-difluoro-2-hydroxybenzoyl)-3-hydroxypyridine O-t-butyloxime (5.19 g) and (E)-2-(4,5-difluoro-2-hydroxybenzoyl)-3-hydroxypyridine O-t-butyloxime (1.49 g) (Compounds 34 and 35).

Aufarbeitung

  1. temperaturecooling to -78° C
  2. additionTo the mixture was added dropwise, under argon atmosphere
  3. stirringby stirring for one hour
  4. customThe cooling bath was removed
  5. stirringthe mixture was stirred for 3 hours
  6. temperaturewhile warming up to room temperature
  7. additionTo the reaction mixture was added ethanol (10 ml)
  8. customto quench
  9. customthe reaction
  10. distillationThe solvent was distilled off under reduced pressure
  11. additionTo the residue were added triethylamine (20 ml), O-t-butylhydroxylamine hydrochloride (3.06 g) and ethanol (50 ml)
  12. temperatureThe mixture was heated for 5 hours
  13. temperatureunder reflux
  14. distillationThe solvent was distilled off
  15. additionTo the residue were added chloroform and water
  16. extractionfor extraction
  17. dry with materialThe organic layer was dried (anhydrous magnesium sulfate)
  18. distillationthe solvent was distilled off under reduced pressure
  19. customThe residue was purified by means of a silica gel column chromatography (eluted with ethyl acetate/hexane)

Quellen und Nachweise

ORD-Eintrag
ord-f23239cda109476a9e87f261484308a8
Quelldatensatz
uspto-grants-1998_02
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US05716971

Notizen zur Reaktion

Wird geladen…

Auf dieser SeiteKomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion