Reaktion #80976

Reaktionsgleichung

1,3-dichloroacetone

N,N-dimethylthiourea

MgSO4

→

desired compound

Ausbeute 70.0%

4-(Chloromethyl)-2-(dimethylamino)thiazole

Ausbeute 70.0%

Lösungsmittel

acetone

acetone

Reaktionsbedingungen

Aufarbeitung

1. 1
   Temperaturwas heated
2. 2
   Temperaturto reflux
3. 3
   TemperaturThe resulting mixture was heated
4. 4
   Temperaturat reflux for 1.5 h
5. 5
   Temperaturto cool
6. 6
   Filtrationfiltered
7. 7
   Einengenconcentrated in vacuo
8. 8
   SonstigeThe residue was purified by silica gel chromatography

Vorschrift

A mixture of 15 g (144 mmol) of N,N-dimethylthiourea and excess MgSO4 in 350 ml of acetone was heated to reflux and treated dropwise with a solution of 18.3 g (144 mmol) of 1,3-dichloroacetone in 35 ml of acetone. The resulting mixture was heated at reflux for 1.5 h, allowed to cool, filtered, and concentrated in vacuo. The residue was purified by silica gel chromatography using 20% ethyl acetate in hexane to provide 14.0 g (70%) of the desired compound.

Quelle