Hydrochloric Acid → 2,7-Bis(4-piperidino-1-buten-1-yl)fluorene

HRID 1576965Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1576965
[N:1]1([CH2:7][CH2:8][CH2:9][CH:10]([C:12]2[CH:24]=[CH:23][C:22]3[C:21]4[C:16](=[CH:17][C:18]([CH:25]([CH2:27][CH2:28][CH2:29][N:30]5[CH2:35][CH2:34][CH2:33][CH2:32][CH2:31]5)O)=[CH:19][CH:20]=4)[CH2:15][C:14]=3[CH:13]=2)O)[CH2:6][CH2:5][CH2:4][CH2:3][CH2:2]1.Cl.C(OCCO)C.[OH-].[Na+]>O>[N:1]1([CH2:7][CH2:8][CH:9]=[CH:10][C:12]2[CH:24]=[CH:23][C:22]3[C:21]4[C:16](=[CH:17][C:18]([CH:25]=[CH:27][CH2:28][CH2:29][N:30]5[CH2:31][CH2:32][CH2:33][CH2:34][CH2:35]5)=[CH:19][CH:20]=4)[CH2:15][C:14]=3[CH:13]=2)[CH2:6][CH2:5][CH2:4][CH2:3][CH2:2]1

Komponenten

6

Edukt 4

HCID 313Hydrochloric AcidHCID 8076Glycol monoethyl etherHCID 14798Sodium HydroxideHCID 5153251-[7-[1-hydroxy-4-(1-piperidyl)butyl]-9H-fluoren-2-yl]-4-(1-piperidyl)butan-1-ol

Produkt 1

HCID 541362442,7-Bis(4-piperidino-1-buten-1-yl)fluorene

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 962WaterLösungsmittel

Reaktionsbedingungen

Temperatur
80 °C

Versuchsvorschrift

A mixture of 4.7 g (0.01 mole) of α,α'-bis(3-piperidinopropyl)-2,7-fluorenedimethanol, 25 ml of concentrated hydrochloric acid and 25 ml of ethylene glycol monoethyl ether is heated at 80°C. for 5 minutes. The solution is diluted with water, made alkaline with a 20% sodium hydroxide solution and the solution is extracted with ether. The ether extract is washed with water, dried over magnesium sulfate and evaporated in vacuo. The residue is crystallized from isopropanol resulting in the preparation of crystalline 2,7-bis(4-piperidino-1-buten-1-yl)fluorene.

Aufarbeitung

  1. extractionthe solution is extracted with ether
  2. extractionThe ether extract
  3. washis washed with water
  4. dry with materialdried over magnesium sulfate
  5. customevaporated in vacuo
  6. customThe residue is crystallized from isopropanol resulting in the preparation of crystalline 2,7-bis(4-piperidino-1-buten-1-yl)fluorene

Quellen und Nachweise

ORD-Eintrag
ord-50733dc07a8d4fe88d0b5fb3faa15cab
Quelldatensatz
uspto-grants-1976_09
Patentnummer
US03983124

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