Dichloromethane → 2-Methylene-3-quinuclidone

HRID 347657

Reaktionsgleichung

Reaktionsgleichung von HRID 347657
Cl.O.O.[CH2:4]=[C:5]1[C:10](=[O:11])[CH:9]2[CH2:12][CH2:13][N:6]1[CH2:7][CH2:8]2.C([O-])([O-])=O.[K+].[K+].C(Cl)Cl>O>[CH2:4]=[C:5]1[C:10](=[O:11])[CH:9]2[CH2:12][CH2:13][N:6]1[CH2:7][CH2:8]2

Komponenten

5

Edukt 3

HCID 6344DichloromethaneHCID 11430Potassium CarbonateHCID 219542752-Methylene-3-quinuclidinone dihydrate hydrochloride

Produkt 1

HCID 3229732-Methylene-3-quinuclidoneAusbeute 100 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 962WaterLösungsmittel

Versuchsvorschrift

A mixture of 2-methylene-3-quinuclidinone dihydrate hydrochloride (27.2 g, 0.13 mol, 1 eq) and K2CO3 (86.0 g, 0.62 mol, 4.8 eq) is dissolved in 130 mL water and 250 mL CH2Cl2 and stirred vigorously. After 3 days, the layers are separated and the aqueous layer is extracted with CH2Cl2. The combined organic layers are dried (MgSO4), filtered and concentrated to give 17.8 g (100%) of 2-methylenequinuclidin3-one as a yellow oil. MS (ESI) for C8H11NO m/z 138.1 (M+).

Aufarbeitung

  1. customthe layers are separated
  2. extractionthe aqueous layer is extracted with CH2Cl2
  3. dry with materialThe combined organic layers are dried (MgSO4)
  4. filtrationfiltered
  5. concentrationconcentrated

Quellen und Nachweise

ORD-Eintrag
ord-97963cac6149420c81d4ebb0fdaae399
Quelldatensatz
uspto-grants-2007_02
Patentnummer
US07176198B2

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