4-Chlorophenyl isothiocyanate → N-(4-chlorophenyl)-3-methylpiperazine-1-carbothioamide

HRID 419846

Reaktionsgleichung

Reaktionsgleichung von HRID 419846
[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([N:8]=[C:9]=[S:10])=[CH:4][CH:3]=1.[CH3:11][CH:12]1[CH2:17][NH:16][CH2:15][CH2:14][NH:13]1>ClCCl>[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([NH:8][C:9]([N:16]2[CH2:15][CH2:14][NH:13][CH:12]([CH3:11])[CH2:17]2)=[S:10])=[CH:4][CH:3]=1

Komponenten

4

Edukt 2

HCID 164804-Chlorophenyl isothiocyanateHCID 660572-Methylpiperazine

Produkt 1

HCID 59347497N-(4-chlorophenyl)-3-methylpiperazine-1-carbothioamide

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6344DichloromethaneLösungsmittel2×

Versuchsvorschrift

A solution of 4-chlorophenyl isothiocyanate (8.0 g, 47.17 mmol) in dichloromethane (250 mL) was added dropwise over 30 minutes to an ice cooled solution of 2-methylpiperazine (9.45 g, 94.33 mmol) in dichloromethane (250 mL). Once the addition was complete, the reaction was stirred at room temperature for an hour. The reaction was then washed with water (3×), dried over MgSO4 and concentrated under reduced pressure, to give the title compound as a white solid, 11.8 g.

Aufarbeitung

  1. additionOnce the addition
  2. washThe reaction was then washed with water (3×)
  3. dry with materialdried over MgSO4
  4. concentrationconcentrated under reduced pressure

Quellen und Nachweise

ORD-Eintrag
ord-c940d342f8f54a50b431f29e56057d8b
Quelldatensatz
uspto-grants-2012_01
Patentnummer
US08093400B2

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