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

Water → 1-(9,9-Di-n-butyl-7-nitrofluorene-2-yl)-ethanone

HRID 630644
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 630644
[CH2:1]([C:5]1([CH2:21][CH2:22][CH2:23][CH3:24])[C:17]2[CH:16]=[C:15]([N+:18]([O-:20])=[O:19])[CH:14]=[CH:13][C:12]=2[C:11]2[C:6]1=[CH:7][CH:8]=[CH:9][CH:10]=2)[CH2:2][CH2:3][CH3:4].[Cl-].[Al+3].[Cl-].[Cl-].[C:29](Cl)(=[O:31])[CH3:30].O>[N+](C1C=CC=CC=1)([O-])=O>[CH2:1]([C:5]1([CH2:21][CH2:22][CH2:23][CH3:24])[C:6]2[CH:7]=[C:8]([C:29](=[O:31])[CH3:30])[CH:9]=[CH:10][C:11]=2[C:12]2[C:17]1=[CH:16][C:15]([N+:18]([O-:20])=[O:19])=[CH:14][CH:13]=2)[CH2:2][CH2:3][CH3:4]
KomponentenReaktionsbedingungenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

6

Edukt 4

HCID 962WaterHCID 6367Acetyl chlorideHCID 6451240Aluminum(III) ChlorideHCID 444715309,9-Dibutyl-2-nitro-9H-fluorene

Produkt 1

HCID 1179383241-(9,9-Di-n-butyl-7-nitrofluorene-2-yl)-ethanoneAusbeute 68,7 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 7416
Nitrobenzene
Lösungsmittel
2×

Reaktionsbedingungen

Temperatur
45 °C

Versuchsvorschrift

After 7.0 g of 9,9-di-n-butyl-2-nitrofluorene (5) (21.7 mmol) was dissolved in 200 ml of anhydrous nitrobenzene and 5.77 g of anhydrous aluminum chloride (43.4 mmol) was added thereto, the reaction mixture was heated to 45° C., and a solution in which 3.40 g of acetyl chloride (43.3 mmol) was dissolved in 40 ml of anhydrous nitrobenzene was slowly added thereto for 1 hour, followed by stirring at 65° C. for 1 hour. Thereafter, the reaction mixture was cooled to room temperature, 100 ml of distilled water was added thereto and stirred for about 30 minutes, followed by extracting the product with 200 ml of dichloromethane. The extracted organic layer was sequentially washed with 100 ml of saturated aqueous sodium bicarbonate solution and 100 ml of distilled water. Then, a solid product obtained by drying the recovered organic layer over anhydrous magnesium sulfate and distilling a solvent under reduced pressure was dispersed in a small amount of ether and stirred at room temperature for 30 minutes, followed by filtering and drying, thereby obtaining 5.44 g of 1-(9,9-di-n-butyl-7-nitrofluorene-2-yl)-ethanone (6) (68.7%) as a light yellow product.

Aufarbeitung

  1. additionwas slowly added
  2. temperatureThereafter, the reaction mixture was cooled to room temperature
  3. stirringstirred for about 30 minutes
  4. extractionby extracting the product with 200 ml of dichloromethane
  5. washThe extracted organic layer was sequentially washed with 100 ml of saturated aqueous sodium bicarbonate solution and 100 ml of distilled water
  6. customThen, a solid product obtained
  7. dry with materialby drying the recovered organic layer over anhydrous magnesium sulfate
  8. distillationdistilling a solvent under reduced pressure
  9. additionwas dispersed in a small amount of ether
  10. stirringstirred at room temperature for 30 minutes
  11. filtrationby filtering
  12. customdrying

Quellen und Nachweise

ORD-Eintrag
ord-9759c8c6ae0c4468b03633c03623c349
Quelldatensatz
uspto-grants-2016_04
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US09316906B2

Notizen zur Reaktion

Wird geladen…

Auf dieser SeiteKomponentenReaktionsbedingungenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion