反応 #95237

反応方程式

sodium

Methylacetate

sodium

Ethyldiethoxyacetate

methylacetate

sodium

→

methyl γ,γ-diethoxyacetoacetate

反応条件

後処理

1. 1
   その他equipped with stirrer
2. 2
   温度reflux condenser
3. 3
   温度heated to reflux
4. 4
   温度heating
5. 5
   workup.DISSOLUTIONis completely dissolved
6. 6
   温度heating
7. 7
   温度The mixture is cooled
8. 8
   抽出the mixture extracted with ether
9. 9
   その他is acidified with hydrochloric acid at 10° C. to 15° C.
10. 10
    抽出the desired product extracted with ether
11. 11
    抽出The ethereal extract
12. 12
    乾燥is dried (Na2SO4)
13. 13
    その他the ether removed
14. 14
    workup.DISTILLATIONthe residue distilled in vacuo

実験手順

Ethyldiethoxyacetate (32 g.) and methylacetate (25 g.) are placed in a flask equipped with stirrer and reflux condenser and heated to reflux. Metallic sodium wire (6.5 g.) is introduced into the flask in small portions and heating continued until the sodium is completely dissolved. Methylacetate (25 g.) and metallic sodium wire (6.5 g.) are then added and heating continued until the solution is clear. The mixture is cooled, a large volume of ice water cautiously added and the mixture extracted with ether. The aqueous solution is acidified with hydrochloric acid at 10° C. to 15° C. and the desired product extracted with ether. The ethereal extract is dried (Na2SO4), the ether removed and the residue distilled in vacuo to give methyl γ,γ-diethoxyacetoacetate.

出典