Benzhydrol → 4-(Diphenylmethoxy)piperidinium chloride

HRID 443802Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 443802
[C:1]1([CH:7]([C:9]2[CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=2)[OH:8])[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.[ClH:15].O[CH:17]1[CH2:22][CH2:21][NH:20][CH2:19][CH2:18]1>C(O)C>[ClH:15].[C:9]1([CH:7]([C:1]2[CH:2]=[CH:3][CH:4]=[CH:5][CH:6]=2)[O:8][CH:17]2[CH2:22][CH2:21][NH:20][CH2:19][CH2:18]2)[CH:10]=[CH:11][CH:12]=[CH:13][CH:14]=1

Komponenten

4

Edukt 2

HCID 7037BenzhydrolHCID 162124994-Hydroxypiperidinium chloride

Produkt 1

HCID 441535184-(Diphenylmethoxy)piperidinium chloride

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 702EthanolLösungsmittel

Versuchsvorschrift

The starting material is prepared as follows: The mixture 268 of diphenylmethanol, 200 g of 4-hydroxypiperidine hydrochloride and 28.8 g of p-toulenesulfonic acid monohydrate is stirred and heated to 160° while reducing the pressure to 0.2 mm Hg with a vacuum pump for 3 hours. It is cooled to 80°, dissolved in 500 ml of ethanol and the solution cooled to 10°. The resulting suspension is filtered, the residue washed with isopropanol and dried at 60°, to yield the 4-diphenylmethoxy-piperidine hydrochloride. It is suspended in 1,800 ml of water, converted into the free base with 125 ml of aqueous ammonia and extracted with diethyl ether and the extract evaporated.

Aufarbeitung

  1. customThe starting material is prepared
  2. temperatureheated to 160°
  3. customfor 3 hours
  4. temperatureIt is cooled to 80°
  5. temperaturethe solution cooled to 10°
  6. filtrationThe resulting suspension is filtered
  7. washthe residue washed with isopropanol
  8. customdried at 60°

Quellen und Nachweise

ORD-Eintrag
ord-49f1418a8e2f4cd698189517829e5e86
Quelldatensatz
uspto-grants-1981_04
Patentnummer
US04261990

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