Dimethyl Sulfate → 1-Methyl-4-phenylpyrrolidin-2-one

HRID 637328

Reaktionsgleichung

Reaktionsgleichung von HRID 637328
[C:1]1([CH:7]2[CH2:11][NH:10][C:9](=[O:12])[CH2:8]2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.S(OC)(O[CH3:17])(=O)=O.[OH-].[Na+]>S([O-])(O)(=O)=O.C([N+](CCCC)(CCCC)CCCC)CCC.C1(C)C=CC=CC=1>[CH3:17][N:10]1[CH2:11][CH:7]([C:1]2[CH:2]=[CH:3][CH:4]=[CH:5][CH:6]=2)[CH2:8][C:9]1=[O:12]

Komponenten

6

Edukt 3

HCID 6497Dimethyl SulfateHCID 14798Sodium HydroxideHCID 1213974-Phenyl-2-pyrrolidinone

Produkt 1

HCID 124489631-Methyl-4-phenylpyrrolidin-2-one

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 94433Tetrabutylammonium hydrogen sulfateKatalysatorHCID 1140TolueneLösungsmittel

Reaktionsbedingungen

Temperatur
36 °C

Versuchsvorschrift

A mixture of 4-phenyl-pyrrolidin-2-one (32.2 g; 0.2 mole), dimethyl sulfate (37.8 g; 0.3 mole), tetrabutyl ammonium hydrogensulfate (3.4 g; 0.01 mole), 50% aqueous sodium hydroxide solution (100 ml) and toluene (200 ml) is stirred at 36° C. for 5 hrs. After cooling, the aqueous phase is decanted, extracted with methylene chloride, and combined with the toluene phase. The organic phase is washed with water, dried and evaporated. The residue is distilled: b.p.0.2 mm Hg =120° C. Yield: 79%.

Aufarbeitung

  1. temperatureAfter cooling
  2. customthe aqueous phase is decanted
  3. extractionextracted with methylene chloride
  4. washThe organic phase is washed with water
  5. customdried
  6. customevaporated
  7. distillationThe residue is distilled
  8. customb.p.0.2 mm Hg =120° C

Quellen und Nachweise

ORD-Eintrag
ord-3e2e03ce5751484982284f4156dbedf2
Quelldatensatz
uspto-grants-1985_12
Patentnummer
US04556674

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