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

Nitric Acid → 1,2,3-Trifluoro-5-methyl-4-nitrobenzene

HRID 424012
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 424012
[F:1][C:2]1[CH:7]=[C:6]([CH3:8])[CH:5]=[C:4]([F:9])[C:3]=1[F:10].[N+:11]([O-])([OH:13])=[O:12]>OS(O)(=O)=O>[F:1][C:2]1[CH:7]=[C:6]([CH3:8])[C:5]([N+:11]([O-:13])=[O:12])=[C:4]([F:9])[C:3]=1[F:10]
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

4

Edukt 2

HCID 944Nitric AcidHCID 177767031,2,3-Trifluoro-5-methylbenzene

Produkt 1

HCID 593863091,2,3-Trifluoro-5-methyl-4-nitrobenzeneAusbeute 85 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 1118Sulfuric AcidLösungsmittel

Versuchsvorschrift

1,2,3-Trifluoro-5-methylbenzene (40 mmol) was added to conc. H2SO4 (50 ml) at 0-5° C. Then the reaction mixture was slowly treated with conc. HNO3 (3.39 ml, 48.44 mmol, 90%) while maintaining the internal temperature below 20° C. The reaction mixture was stirred at room temperature for 16 h and poured onto ice (300 g) and the oily layer was extracted with CH2Cl2 (2×125 ml). The organic layer was washed with water (2×200 ml), brine (200 ml) and dried (MgSO4) and evaporated to obtain the crude product which was purified over flash silica gel chromatography to obtain the title product (6.5 g, 85%). 1H-NMR (300 MHz, CDCl3): δ 6.96 (septet, 1H), 2.39 (s, 3H). 19FNMR (CDCl3): δ −128.18, −141.50, −159.05.

Aufarbeitung

  1. temperaturewhile maintaining the internal temperature below 20° C
  2. additionpoured onto ice (300 g)
  3. extractionthe oily layer was extracted with CH2Cl2 (2×125 ml)
  4. washThe organic layer was washed with water (2×200 ml), brine (200 ml)
  5. dry with materialdried (MgSO4)
  6. customevaporated
  7. customto obtain the crude product which
  8. customwas purified over flash silica gel chromatography

Quellen und Nachweise

ORD-Eintrag
ord-ef6679938b5c438391d5f93f7de26a58
Quelldatensatz
uspto-grants-2012_01
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US08101799B2

Notizen zur Reaktion

Wird geladen…

Auf dieser SeiteKomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion