Reaktion #2941

Reaktionsgleichung

ethyl acetoacetate

i-butyl alcohol

p-toluensulphonic acid

→

title compound

i-Butyl acetoacetate

Reaktionsbedingungen

Aufarbeitung

1. 1
   TemperaturThe solution was refluxed for 18 h
2. 2
   SonstigeThe reaction mixture was evaporated in vacuo
3. 3
   workup.DISSOLUTIONthe residue was dissolved in ether
4. 4
   workup.ADDITIONThe resulted solution was treated with s.s
5. 5
   SonstigeThe organic layer was separated
6. 6
   Trocknendried over Na2SO4
7. 7
   Sonstigeevaporated in vacuo
8. 8
   workup.DISTILLATIONThe crude oil was distilled at 66°-68° C./4 mmHg

Vorschrift

30 ml of ethyl acetoacetate were dissolved in 350 ml of i-butyl alcohol and a catalytic amount of p-toluensulphonic acid (PTSA) was added. The solution was refluxed for 18 h. The reaction mixture was evaporated in vacuo and the residue was dissolved in ether. The resulted solution was treated with s.s. NaHCO3. The organic layer was separated, dried over Na2SO4 and evaporated in vacuo. The crude oil was distilled at 66°-68° C./4 mmHg, to give 18.8 g of the title compound.

Quelle