Реакция #2941

Уравнение реакции

ethyl acetoacetate

i-butyl alcohol

p-toluensulphonic acid

→

title compound

i-Butyl acetoacetate

Условия реакции

Обработка

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

Методика

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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