반응 #95237

반응 방정식

sodium

Methylacetate

sodium

Ethyldiethoxyacetate

methylacetate

sodium

→

methyl γ,γ-diethoxyacetoacetate

반응 조건

후처리

1. 1
   기타equipped with stirrer
2. 2
   온도reflux condenser
3. 3
   온도heated to reflux
4. 4
   온도heating
5. 5
   workup.DISSOLUTIONis completely dissolved
6. 6
   온도heating
7. 7
   온도The mixture is cooled
8. 8
   추출the mixture extracted with ether
9. 9
   기타is acidified with hydrochloric acid at 10° C. to 15° C.
10. 10
    추출the desired product extracted with ether
11. 11
    추출The ethereal extract
12. 12
    건조is dried (Na2SO4)
13. 13
    기타the ether removed
14. 14
    workup.DISTILLATIONthe residue distilled in vacuo

실험 절차

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.

출처