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

Hydroxylamine → 7,7-Di-pyridin-2-yl-hept-6-enoic acid hydroxyamide

HRID 404133
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 404133
[OH:1][NH2:2].[N:3]1[CH:8]=[CH:7][CH:6]=[CH:5][C:4]=1[C:9]([C:18]1[CH:23]=[CH:22][CH:21]=[CH:20][N:19]=1)=[CH:10][CH2:11][CH2:12][CH2:13][CH2:14][C:15](O)=[O:16].CCOC(C)=O>CN(C=O)C.C1COCC1.[Cl-].[Na+].O>[OH:1][NH:2][C:15](=[O:16])[CH2:14][CH2:13][CH2:12][CH2:11][CH:10]=[C:9]([C:18]1[CH:23]=[CH:22][CH:21]=[CH:20][N:19]=1)[C:4]1[CH:5]=[CH:6][CH:7]=[CH:8][N:3]=1
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

7

Edukt 3

HCID 787HydroxylamineHCID 8857Ethyl AcetateHCID 585450627,7-Di-pyridin-2-yl-hept-6-enoic acid

Produkt 1

HCID 468523047,7-Di-pyridin-2-yl-hept-6-enoic acid hydroxyamide

Reagenzien, Katalysatoren, Lösungsmittel 3

HCID 6228DimethylformamideLösungsmittelHCID 8028
Tetrahydrofuran
Lösungsmittel
HCID 57417360Sodium chloride; waterLösungsmittel

Versuchsvorschrift

HONH2 (50% aqueous, 0.3 mL) was added to IV (32 mg, 0.1 mmol) in DMF (0.3 mL) and THF (0.3 mL) at 0° C. The reaction mixture was stirred at it for 17 h, after which brine (3 mL) and EtOAc (3 mL) were added. The phases were separated, and the aqueous phase was extracted with EtOAc (2×3 mL). The organic phases were then combined, dried over MgSO4, filtered, and subsequently evaporated under reduced pressure. The resulting residue was purified by silica gel column chromatography using CH2Cl2/MeOH (100:3 to 100:10) as eluant to furnish V, a colourless oil (9.6 mg, 30%).

Aufarbeitung

  1. customThe phases were separated
  2. extractionthe aqueous phase was extracted with EtOAc (2×3 mL)
  3. dry with materialdried over MgSO4
  4. filtrationfiltered
  5. customsubsequently evaporated under reduced pressure
  6. customThe resulting residue was purified by silica gel column chromatography
  7. customto furnish V

Quellen und Nachweise

ORD-Eintrag
ord-3c2a8810ba2f4e9ea9b6eee5b715666b
Quelldatensatz
uspto-grants-2014_06
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US08748458B2

Notizen zur Reaktion

Wird geladen…

Auf dieser SeiteKomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion