Reaktion #214666

Reaktionsgleichung

dichloroacetyl chloride

4-methyl-cyclohexanone

ethanolamine

pyridine

→

product

N-dichloroacetyl-8-methyl-1-oxa-4-azaspiro[4,5]decane

Reaktionsbedingungen

Aufarbeitung

1. 1
   workup.ADDITIONFrom a boiling mixture of 11.2 g
2. 2
   workup.DISTILLATIONof benzene the formed water is continuously distilled off
3. 3
   Sonstigeof water are separated
4. 4
   TemperaturThe reaction mixture is then cooled
5. 5
   workup.ADDITIONfollowed by dropwise addition of 14.7 g
6. 6
   Sonstigeoily product are obtained
7. 7
   SonstigeRecrystallization from absolute ethanol

Vorschrift

From a boiling mixture of 11.2 g. (0.1 moles) of 4-methyl-cyclohexanone and 6.1 g. (0.1 moles) of ethanolamine in 100 ml. of benzene the formed water 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 dropwise addition of 14.7 g. (0.1 moles) of dichloroacetyl chloride with external salt/ice cooling. Further following the procedure described in Example 2, 20.7 g. (0.078 moles) of a rose, oily product are obtained. Recrystallization from absolute ethanol affords a white, crystalline product melting at 119° to 120° C. The structure of the compound obtained can be verified by IR spectrum analysis.

Quelle