반응 #2941

반응 방정식

ethyl acetoacetate

i-butyl alcohol

p-toluensulphonic acid

→

title compound

i-Butyl acetoacetate

반응 조건

후처리

1. 1
   온도The solution was refluxed for 18 h
2. 2
   기타The 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
   기타The organic layer was separated
6. 6
   건조dried over Na2SO4
7. 7
   기타evaporated in vacuo
8. 8
   workup.DISTILLATIONThe crude oil was distilled at 66°-68° C./4 mmHg

실험 절차

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.

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