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Hydrochloric Acid → HCID 13799019, Verbindung

HRID 255880
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Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 255880
Cl[CH:2]1[C:10]2[C:5](=[C:6]([O:11][CH3:12])[CH:7]=[CH:8][CH:9]=2)[CH2:4][CH2:3]1.[NH:13]1[CH2:18][CH2:17][CH2:16][CH2:15][CH2:14]1.Cl>C(Cl)(Cl)Cl>[CH3:12][O:11][C:6]1[CH:7]=[CH:8][CH:9]=[C:10]2[C:5]=1[CH2:4][CH2:3][CH:2]2[N:13]1[CH2:18][CH2:17][CH2:16][CH2:15][CH2:14]1
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

5

Edukt 3

HCID 313Hydrochloric AcidHCID 8082PiperidineHCID 13799018HCID 13799018, Verbindung

Produkt 1

HCID 13799019HCID 13799019, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6212ChloroformLösungsmittel2×

Versuchsvorschrift

A solution of 1-chloro-4-methoxyindan (from Step 3) in chloroform (130 ml) is added over a period of ten minutes to a stirred mixture of piperidine (284 ml) in chloroform (400 ml) under nitrogen. The reaction mixture is heated to reflux for six hours and allowed to stand at RT overnight. The mixture is treated with 10% aqueous HCl and the organic layer separated. The aqueous layer is extracted with methylene chloride and the combined organic extracts washed with 10% aqueous HCl. The organic layer is evaporated in vacuo and the residue partitioned between 5% aqueous HCl and ether. The combined aqueous fraction is washed with ether, made alkaline, and the alkaline layer extracted with ether. The ether extract is washed, dried and concentrated in vacuo yielding the piperidine indan as an oil.

Aufarbeitung

  1. temperatureThe reaction mixture is heated
  2. temperatureto reflux for six hours
  3. customthe organic layer separated
  4. extractionThe aqueous layer is extracted with methylene chloride
  5. washthe combined organic extracts washed with 10% aqueous HCl
  6. customThe organic layer is evaporated in vacuo
  7. customthe residue partitioned between 5% aqueous HCl and ether
  8. washThe combined aqueous fraction is washed with ether
  9. extractionthe alkaline layer extracted with ether
  10. extractionThe ether extract
  11. washis washed
  12. customdried
  13. concentrationconcentrated in vacuo

Quellen und Nachweise

ORD-Eintrag
ord-d7454a20d96343bfb90046ef3ef9afa8
Quelldatensatz
uspto-grants-1987_10
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US04699906

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