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

HRID 20275

Reaktionsgleichung

Reaktionsgleichung von HRID 20275
[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-5f9a14faca964707886135ffa8096e54
Quelldatensatz
uspto-grants-2010_06
Patentnummer
US07745630B2

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