4-Chlorobenzylamine hydrochloride → HCID 178512103, Verbindung

HRID 413748

Reaktionsgleichung

Reaktionsgleichung von HRID 413748
[NH:1]([C:4]1[CH:5]=[C:6]([C:10]([F:13])([F:12])[F:11])[CH:7]=[CH:8][CH:9]=1)[C:2]#[N:3].Cl.[Cl:15][C:16]1[CH:23]=[CH:22][C:19]([CH2:20][NH2:21])=[CH:18][CH:17]=1>ClCCl>[Cl:15][C:16]1[CH:23]=[CH:22][C:19]([CH2:20][NH:21][C:2]([NH:1][C:4]2[CH:9]=[CH:8][CH:7]=[C:6]([C:10]([F:11])([F:12])[F:13])[CH:5]=2)=[NH:3])=[CH:18][CH:17]=1

Komponenten

4

Edukt 2

HCID 4584434-Chlorobenzylamine hydrochlorideHCID 110741023-(Trifluoromethyl)phenylcyanamide

Produkt 1

HCID 178512103HCID 178512103, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6344DichloromethaneLösungsmittel

Reaktionsbedingungen

Temperatur
150 °C

Versuchsvorschrift

A mixture of 3-cyanamidobenzotrifluoride (1.20 g, 6.45 mmol) and 4-chlorobenzylamine hydrochloride (1.26 g, 7.09 mmol) was stirred at 150° C. for 40 h. Dichloromethane (100 ml) was added and the mixture was washed with saturated aqueous sodium hydrogen carbonate (100 ml). The organic phase was purified by chromatography using silica gel and a mixture of methanol (10%) and dichloromethane as eluent. The product was isolated as the free base. Yield 1.05 g, 50%. M.p. 103-105° C.

Aufarbeitung

  1. washthe mixture was washed with saturated aqueous sodium hydrogen carbonate (100 ml)
  2. customThe organic phase was purified by chromatography
  3. additiona mixture of methanol (10%) and dichloromethane as eluent
  4. customThe product was isolated as the free base

Quellen und Nachweise

ORD-Eintrag
ord-c8effcddc3a642b88b36d357be4d8d7d
Quelldatensatz
uspto-grants-2003_05
Patentnummer
US06569880B2

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