Reaktion #80967

Reaktionsgleichung

2-methylpropane-thioamide

1,3-dichloroacetone

MgSO4

→

crude desired compound

4-(Chloromethyl)-2-isopropylthiazole hydrochloride

Lösungsmittel

acetone

Reaktionsbedingungen

Aufarbeitung

1. 1
   Temperaturwas heated
2. 2
   Temperaturat reflux for 3.5 h
3. 3
   Temperaturto cool
4. 4
   Filtrationfiltered
5. 5
   Sonstigethe solvent was removed in vacuo

Vorschrift

A mixture of 94.0 g (0.91 mol) of 2-methylpropane-thioamide, 115.7 g (0.91 mol) of 1,3-dichloroacetone, and 109.7 g (0.91 mol) of MgSO4 in 1.6 liters of acetone was heated at reflux for 3.5 h. The resulting mixture was allowed to cool, filtered, and the solvent was removed in vacuo to provide the crude desired compound as a yellow oil. 1H NMR (DMSO-d6) δ1.32 (d, J=7 Hz, 6H), 3.27 (heptet, J=7 Hz, 1H), 4.78 (s, 2H), 7.61 (s, 1H). Mass spectrum: (M+H)+ =176.

Quelle