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

HRID 481960Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 481960
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-1fce0c99b5004278a4e334282a24e19d
Quelldatensatz
uspto-grants-1998_08
Patentnummer
US05792768

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