4-Chlorobenzylamine hydrochloride → HCID 178512103, Verbindung

HRID 843584Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 843584
[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-f4125f66025649098824247548b31a4c
Quelldatensatz
uspto-grants-2002_04
Patentnummer
US06380180B1

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