Reaktion #214668

Reaktionsgleichung

dichloroacetyl chloride

cyclopentanone

2-mercaptoethylamine

pyridine

→

N-dichloroacetyl-1-thia-4-azaspiro[4,4]nonane

Lösungsmittel

water

benzene

Reaktionsbedingungen

Aufarbeitung

1. 1
   workup.ADDITIONFrom a boiling mixture of 8.4 g
2. 2
   workup.DISTILLATIONis continuously distilled off
3. 3
   Sonstigeof water are separated
4. 4
   TemperaturThe reaction mixture is then cooled
5. 5
   workup.ADDITIONfollowed by a dropwise addition of 14.7 g

Vorschrift

From a boiling mixture of 8.4 g. (0.1 moles) of cyclopentanone and 7.7 g. (0.1 mole) of 2-mercaptoethylamine in 100 ml. of benzene the water formed is continuously distilled off. Boiling is continued until 1.8 ml. of water are separated. The reaction mixture is then cooled and 8 g. (0.1 moles) of pyridine are added followed by a dropwise addition of 14.7 g. (0.1 moles) of dichloroacetyl chloride, with external salt/ice cooling.

Quelle