Potassium Hydroxide → 4-(3,4-Dichlorophenyl)-4-piperidinol

HRID 1886160Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1886160
C(OC([N:6]1[CH2:11][CH2:10][C:9]([OH:20])([C:12]2[CH:17]=[CH:16][C:15]([Cl:18])=[C:14]([Cl:19])[CH:13]=2)[CH2:8][CH2:7]1)=O)C.[OH-].[K+]>C(O)CCC>[OH:20][C:9]1([C:12]2[CH:17]=[CH:16][C:15]([Cl:18])=[C:14]([Cl:19])[CH:13]=2)[CH2:10][CH2:11][NH:6][CH2:7][CH2:8]1

Komponenten

4

Edukt 2

HCID 14797Potassium HydroxideHCID 20077503Ethyl 4-(3,4-dichlorophenyl)-4-hydroxypiperidine-1-carboxylate

Produkt 1

HCID 186757284-(3,4-Dichlorophenyl)-4-piperidinolAusbeute 90 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 2631-ButanolLösungsmittel

Versuchsvorschrift

A mixture of 64.2 g of 1-ethoxycarbonyl-4-hydroxy-4-(3,4-dichlorophenyl)piperidine (X-1) and a solution of 72.4 g of KOH in 700 ml of nBuOH is refluxed for 2 hours and evaporated. The reaction mixture is concentrated under reduced pressure and extracted with ethyl acetate. The organic layer is washed with water, dried and evaporated. The resulting crystalline residue is recrystallized from ethyl acetate to prepare 44.7 g (Yield: 90.0%) of the compound (II-1). mp. 144.5°-146.0° C.

Aufarbeitung

  1. customevaporated
  2. concentrationThe reaction mixture is concentrated under reduced pressure
  3. extractionextracted with ethyl acetate
  4. washThe organic layer is washed with water
  5. customdried
  6. customevaporated
  7. customThe resulting crystalline residue is recrystallized from ethyl acetate

Quellen und Nachweise

ORD-Eintrag
ord-5489b2fcd6ac41ec9ee9a1619c198797
Quelldatensatz
uspto-grants-1992_09
Patentnummer
US05149817

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