Dichloromethane → 7-tert-Butyl-1-methylpyrene

HRID 1914410Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1914410
[CH3:1][C:2]1[C:15]2[C:16]3=[C:17]4[C:12](=[CH:13][CH:14]=2)[CH:11]=[CH:10][CH:9]=[C:8]4[CH:7]=[CH:6][C:5]3=[CH:4][CH:3]=1.[C:18](Cl)([CH3:21])([CH3:20])[CH3:19].ClCCl.[Cl-].[Al+3].[Cl-].[Cl-]>O>[C:18]([C:10]1[CH:9]=[C:8]2[C:17]3=[C:16]4[C:5](=[CH:4][CH:3]=[C:2]([CH3:1])[C:15]4=[CH:14][CH:13]=[C:12]3[CH:11]=1)[CH:6]=[CH:7]2)([CH3:21])([CH3:20])[CH3:19]

Komponenten

6

Edukt 4

HCID 6344DichloromethaneHCID 10486tert-BUTYL CHLORIDEHCID 169321-MethylpyreneHCID 6451240Aluminum(III) Chloride

Produkt 1

HCID 30866837-tert-Butyl-1-methylpyreneAusbeute 54,1 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 962WaterLösungsmittel

Versuchsvorschrift

Next, a mixed solution of 4.4 g of 1-methylpyrene, 2 g of t-butylchloride and 33 ml of dichloromethane was cooled to 0° C. under a nitrogen gas stream and then 2.7 g of aluminum chloride was added. This mixed solution was stirred at room temperature for 3 hours and 30 ml of water was poured into the solution, followed by extraction with 30 ml of dichloromethane. The organic layer was washed twice with 20 ml of water, dried over magnesium sulfate and then evaporated. The concentrate was purified by silica gel column chromatography and then vacuum-dried to obtain 3 g of 7-t-butyl-1-methylpyrene.

Aufarbeitung

  1. extractionfollowed by extraction with 30 ml of dichloromethane
  2. washThe organic layer was washed twice with 20 ml of water
  3. dry with materialdried over magnesium sulfate
  4. customevaporated
  5. customThe concentrate was purified by silica gel column chromatography
  6. customvacuum-dried

Quellen und Nachweise

ORD-Eintrag
ord-ae6368f67b7047a489bc72fcffdf2610
Quelldatensatz
uspto-grants-2013_12
Patentnummer
US08610345B2

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