1-Chloroethyl chloroformate → 1-(Benzothiophen-2-yl)piperazine hydrochloride

HRID 1900560Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1900560
C([N:8]1[CH2:13][CH2:12][N:11]([C:14]2[S:15][C:16]3[CH:22]=[CH:21][CH:20]=[CH:19][C:17]=3[CH:18]=2)[CH2:10][CH2:9]1)C1C=CC=CC=1.[Cl:23]C(OC(Cl)=O)C>ClCCl>[ClH:23].[S:15]1[C:16]2[CH:22]=[CH:21][CH:20]=[CH:19][C:17]=2[CH:18]=[C:14]1[N:11]1[CH2:12][CH2:13][NH:8][CH2:9][CH2:10]1

Komponenten

4

Edukt 2

HCID 5213051-Chloroethyl chloroformateHCID 217016231-Benzyl-4-(benzothiophen-2-yl)piperazine

Produkt 1

HCID 190649731-(Benzothiophen-2-yl)piperazine hydrochloride

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6344DichloromethaneLösungsmittel

Versuchsvorschrift

To a solution of 1-benzyl-4-(benzothiophen-2-yl)piperazine (1.5 g, 4.9 mmol) in anhydrous dichloromethane (20 ml) at 0° C. under nitrogen was added 1-chloroethylchloroformate (0.68 ml, 6.37 mmol). The mixture was allowed to warm to room temperature, stirred for 1 h and concentrated in vacuo. The crude residue was dissolved in methanol (10 ml) and heated to reflux for 30 minutes, left to cool and the title compound collected by filtration (0.6 g), m.p. 240° C. (dec.).

Aufarbeitung

  1. concentrationconcentrated in vacuo
  2. dissolutionThe crude residue was dissolved in methanol (10 ml)
  3. temperatureheated
  4. temperatureto reflux for 30 minutes
  5. waitleft
  6. temperatureto cool
  7. filtrationthe title compound collected by filtration (0.6 g), m.p. 240° C. (dec.)

Quellen und Nachweise

ORD-Eintrag
ord-67a08c733cb949368f22a3192202c0ff
Quelldatensatz
uspto-grants-1996_11
Patentnummer
US05576319

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