Ethyl chloroformate → Ethyl 3-methyl-4-oxopiperidine-1-carboxylate

HRID 486436

Reaktionsgleichung

Reaktionsgleichung von HRID 486436
[CH3:1][CH:2]1[C:7](=[O:8])[CH2:6][CH2:5][N:4](CC2C=CC=CC=2)[CH2:3]1.[C:16](Cl)(=[O:20])[O:17][CH2:18][CH3:19]>CC1C=CC=CC=1>[CH3:1][CH:2]1[C:7](=[O:8])[CH2:6][CH2:5][N:4]([C:16]([O:17][CH2:18][CH3:19])=[O:20])[CH2:3]1

Komponenten

4

Edukt 2

HCID 10928Ethyl chloroformateHCID 5609651-Benzyl-3-methyl-4-piperidone

Produkt 1

HCID 15075657Ethyl 3-methyl-4-oxopiperidine-1-carboxylateAusbeute 83 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 1140TolueneLösungsmittel

Versuchsvorschrift

To a stirred solution of 152 parts of 3-methyl-1-(phenylmethyl)-4-piperidinone in 900 parts of methylbenzene were added dropwise 218 parts of ethyl carbonochloridate at room temperature. Upon completion, stirring was continued overnight at reflux. After cooling, the reaction mixture was washed with water and hydrochloric acid, dried, filtered and evaporated. The residue was distilled, yielding 120.5 parts (83%) of ethyl 3-methyl-4-oxo-1-piperidinecarboxylate; bp. 98°-105° C. at 1 mm pressure (intermediate 26).

Aufarbeitung

  1. temperatureat reflux
  2. temperatureAfter cooling
  3. washthe reaction mixture was washed with water and hydrochloric acid
  4. customdried
  5. filtrationfiltered
  6. customevaporated
  7. distillationThe residue was distilled

Quellen und Nachweise

ORD-Eintrag
ord-abcf0f1d31534ab2b8f0fd36767139f3
Quelldatensatz
uspto-grants-1994_03
Patentnummer
US05292738

Verknüpfte Notizen

Wird geladen…