Reaktion #302892

ord-ab661d7a8bcc4d6ba081a13baa6c3320

Reaktionsgleichung

Cc1cccc(CN)c1C
2,3-dimethylbenzylamine
S=C=NCCCl
2-chloroethylisothiocyanate
Cc1cccc(CNC2=NCCS2)c1C.Cl
title compound
Ausbeute 76.0%
Cc1cccc(CNC2=NCCS2)c1C.Cl
((2,3-dimethylphenyl)methyl)-1,3-thiazolin-2-ylamine hydrochloride
Ausbeute 76.0%

Lösungsmittel

Reaktionsbedingungen

Temperatur
80°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Temperaturto cool
  2. 2
    Sonstigea solid precipitate that had formed
  3. 3
    Filtrationwas collected by filtration
  4. 4
    WaschenThe solid was rinsed with diethyl ether
  5. 5
    Sonstigewas dried under reduced pressure

Vorschrift

Under a dry nitrogen atmosphere, a stirred mixture of 5.56 grams (0.041 mole) of 2,3-dimethylbenzylamine and 5.0 grams (0.041 mole) of 2-chloroethylisothiocyanate in 100 mL of 1,4-dioxane was heated to 80° C. where it stirred for about 18 hours. The reaction mixture was allowed to cool and a solid precipitate that had formed was collected by filtration. The solid was rinsed with diethyl ether and was dried under reduced pressure to yield 8.0 grams of the title compound. The NMR spectrum was consistent with the proposed structure.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US08193118B2uspto-grants-2012_06