反応 #2941

反応方程式

ethyl acetoacetate

i-butyl alcohol

p-toluensulphonic acid

→

title compound

i-Butyl acetoacetate

反応条件

後処理

1. 1
   温度The solution was refluxed for 18 h
2. 2
   その他The 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
   その他The organic layer was separated
6. 6
   乾燥dried over Na2SO4
7. 7
   その他evaporated in vacuo
8. 8
   workup.DISTILLATIONThe crude oil was distilled at 66°-68° C./4 mmHg

実験手順

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.

出典