Sodium Carbonate → 1-(5,6,7,8-Tetrahydronaphthalen-1-yl)piperazine

HRID 481353

Reaktionsgleichung

Reaktionsgleichung von HRID 481353
[C:1]1([NH2:11])[C:10]2[CH2:9][CH2:8][CH2:7][CH2:6][C:5]=2[CH:4]=[CH:3][CH:2]=1.Cl.Cl[CH2:14][CH2:15][NH:16][CH2:17][CH2:18]Cl.C(=O)([O-])[O-].[Na+].[Na+]>C(O)CCC>[C:1]1([N:11]2[CH2:18][CH2:17][NH:16][CH2:15][CH2:14]2)[C:10]2[CH2:9][CH2:8][CH2:7][CH2:6][C:5]=2[CH:4]=[CH:3][CH:2]=1

Komponenten

5

Edukt 3

HCID 10340Sodium CarbonateHCID 166715-TetralinylamineHCID 522769Bis(2-chloroethyl)amine hydrochloride

Produkt 1

HCID 986981-(5,6,7,8-Tetrahydronaphthalen-1-yl)piperazine

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 2631-ButanolLösungsmittel

Versuchsvorschrift

5,6,7,8-Tetrahydronaphthalen-1-ylamine (1.4 ml, 15 mmol) is brought to the reflux point of 1-butanol (50 ml) in the presence of bis(2-chloroethyl)amine hydrochloride (2.68 g, 15 mmol) and sodium carbonate (800 mg, 7.5 mmol). After 48 h, the reaction mixture is concentrated and impregnated onto silica and then purified by flash chromatography with a mixture (95/5/1) and then (90/9/1) of dichloromethane/methanol/aqueous ammonia.

Aufarbeitung

  1. concentrationthe reaction mixture is concentrated
  2. custompurified by flash chromatography with a mixture (95/5/1)

Quellen und Nachweise

ORD-Eintrag
ord-cf5b8c9e07c747c3ac0fadf998fe5196
Quelldatensatz
uspto-grants-1998_08
Patentnummer
US05789412

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