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

Nitric Acid → HCID 86686556, Verbindung

HRID 1528067
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 1528067
[F:1][C:2]1[CH:10]=[CH:9][CH:8]=[C:7]2[C:3]=1[C:4]([CH3:13])([CH3:12])[C:5](=[O:11])[NH:6]2.[N+:14]([O-])([OH:16])=[O:15]>S(=O)(=O)(O)O>[F:1][C:2]1[C:10]([N+:14]([O-:16])=[O:15])=[CH:9][CH:8]=[C:7]2[C:3]=1[C:4]([CH3:13])([CH3:12])[C:5](=[O:11])[NH:6]2
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

4

Edukt 2

HCID 944Nitric AcidHCID 248243364-Fluoro-3,3-dimethyl-1,3-dihydro-2H-indol-2-one

Produkt 1

HCID 86686556HCID 86686556, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 1118Sulfuric AcidLösungsmittel2×

Versuchsvorschrift

To a solution of 4-fluoro-3,3-dimethyl-1,3-dihydro-2H-indol-2-one (4.1 g) in concentrated sulfuric acid (60 mL) was added dropwise a mixture of fuming nitric acid (0.99 mL) and concentrated sulfuric acid (10 mL) over 30 min at −30° C. The reaction mixture was stirred between −30° C. to 0° C. for 30 min, and poured into ice. The resulting solid was collected by filtration, washed with water, and dissolved in ethyl acetate. The obtained solution was washed with water and saturated brine, dried over anhydrous magnesium sulfate, and concentrated under reduced pressure. The obtained residue was purified by silica gel column chromatography (ethyl acetate/hexane) to give the title compound (2.2 g).

Aufarbeitung

  1. additionpoured into ice
  2. filtrationThe resulting solid was collected by filtration
  3. washwashed with water
  4. dissolutiondissolved in ethyl acetate
  5. washThe obtained solution was washed with water and saturated brine
  6. dry with materialdried over anhydrous magnesium sulfate
  7. concentrationconcentrated under reduced pressure
  8. customThe obtained residue was purified by silica gel column chromatography (ethyl acetate/hexane)

Quellen und Nachweise

ORD-Eintrag
ord-edeea989b2344b3ca00cc625e82c097a
Quelldatensatz
uspto-grants-2015_07
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US09090586B2

Notizen zur Reaktion

Wird geladen…

Auf dieser SeiteKomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion