2-Bromo-2-methylpropionyl bromide → HCID 71089296, Verbindung

HRID 1055281Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1055281
[CH2:1]([C:7]1([CH2:20][CH2:21][CH2:22][CH2:23][CH2:24][CH3:25])[C:19]2[CH:18]=[CH:17][CH:16]=[CH:15][C:14]=2[C:13]2[C:8]1=[CH:9][CH:10]=[CH:11][CH:12]=2)[CH2:2][CH2:3][CH2:4][CH2:5][CH3:6].Br[C:27]([CH3:32])([CH3:31])[C:28](Br)=[O:29].[Cl-].[Cl-].[Cl-].[Al+3]>C(=S)=S>[CH2:20]([C:7]1([CH2:1][CH2:2][CH2:3][CH2:4][CH2:5][CH3:6])[C:19]2[CH:18]=[C:17]3[C:28](=[O:29])[CH:27]([CH3:32])[CH2:31][C:16]3=[CH:15][C:14]=2[C:13]2[C:8]1=[CH:9][CH:10]=[CH:11][CH:12]=2)[CH2:21][CH2:22][CH2:23][CH2:24][CH3:25]

Komponenten

5

Edukt 3

HCID 886852-Bromo-2-methylpropionyl bromideHCID 51284499,9-dihexylfluoreneHCID 6451240Aluminum(III) Chloride

Produkt 1

HCID 71089296HCID 71089296, VerbindungAusbeute 93,6 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6348Carbon DisulfideLösungsmittel

Versuchsvorschrift

9,9-dihexyl-9H-fluorene (79 g, 236.2 mmol) and 2-bromo-2-methylpropanoyl bromide (54.3 g, 236.2 mmol) were injected into a 2000 mL round flask and then dissolved by adding 600 mL of carbon disulfide inputted thereto. Then, the reactor was cooled with ice water. Aluminum trichloride (78.7 g, 590.4 mmol) was slowly added thereto in ten lots over 2 hours under nitrogen atmosphere. Then, after the mixture was stirred at room temperature for 8 hours, the reaction was terminated by adding of 500 mL of distilled water, followed by washing with 500 mL of distilled water three times. The organic layer was dried over magnesium sulfate, followed by removal of volatile materials and drying, thereby obtaining 89.0 g of 9,9-dihexyl-2-methyl-2,3-dihydrocyclopenta[b]fluoren-1(9H)-one (yield: 93.6%) as highly viscous oil.

Aufarbeitung

  1. dissolutiondissolved
  2. customthe reaction was terminated
  3. additionby adding of 500 mL of distilled water
  4. washby washing with 500 mL of distilled water three times
  5. dry with materialThe organic layer was dried over magnesium sulfate
  6. customfollowed by removal of volatile materials
  7. customdrying

Quellen und Nachweise

ORD-Eintrag
ord-7e63d456170148a4ab568bdc32750bd4
Quelldatensatz
uspto-grants-2016_07
Patentnummer
US09394388B2

Notizen zur Reaktion

Wird geladen…