Methyl Ethyl Ketone → 6-Methyl-6-ethylfulvene

HRID 270994Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 270994
[CH:1]1[CH2:5][CH:4]=[CH:3][CH:2]=1.[CH2:6]([C:8]([CH3:10])=O)[CH3:7].N1CCCC1>CO.CCOCC.O>[CH3:7][C:6]([CH2:8][CH3:10])=[C:2]1[CH:1]=[CH:5][CH:4]=[CH:3]1

Komponenten

7

Edukt 3

HCID 6569Methyl Ethyl KetoneHCID 7612CyclopentadieneHCID 31268Pyrrolidine

Produkt 1

HCID 5707046-Methyl-6-ethylfulveneAusbeute 51 %

Reagenzien, Katalysatoren, Lösungsmittel 3

HCID 887MethanolLösungsmittelHCID 962WaterLösungsmittelHCID 3283Diethyl EtherLösungsmittel

Versuchsvorschrift

To a solution of 10.00 g (151.3 mmol) of cyclopentadiene in 30 ml of methanol, 13.6 ml (151.8 mmol) of methyl ethyl ketone and 12.8 ml (153.3 mmol) of pyrrolidine were added with ice cooling, followed by stirring at room temperature for one night. After the reaction solution was diluted with 200 ml of ether, 100 ml of water was added. The organic phase was separated, washed with water and a saturated saline solution, then dried over anhydrous magnesium sulfate and filtered. From the filtrate, the solvent was removed under reduced pressure to obtain a liquid. The liquid was subjected to vacuum distillation (75-82° C./20 mmHg) to obtain 9.20 g (76.55 mmol) of a yellow liquid (yield: 51%). The analyzed values are given below.

Aufarbeitung

  1. additionwas added
  2. customThe organic phase was separated
  3. washwashed with water
  4. dry with materiala saturated saline solution, then dried over anhydrous magnesium sulfate
  5. filtrationfiltered
  6. customFrom the filtrate, the solvent was removed under reduced pressure
  7. customto obtain a liquid
  8. distillationThe liquid was subjected to vacuum distillation (75-82° C./20 mmHg)

Quellen und Nachweise

ORD-Eintrag
ord-c41c6f5e84a74e9c80394e84ebe81a18
Quelldatensatz
uspto-grants-2008_11
Patentnummer
US07449533B2

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