تفاعل #95237

معادلة التفاعل

sodium

Methylacetate

sodium

Ethyldiethoxyacetate

methylacetate

sodium

→

methyl γ,γ-diethoxyacetoacetate

ظروف التفاعل

المعالجة

1. 1
   أخرىequipped with stirrer
2. 2
   درجة الحرارةreflux condenser
3. 3
   درجة الحرارةheated to reflux
4. 4
   درجة الحرارةheating
5. 5
   workup.DISSOLUTIONis completely dissolved
6. 6
   درجة الحرارةheating
7. 7
   درجة الحرارةThe mixture is cooled
8. 8
   استخلاصthe mixture extracted with ether
9. 9
   أخرىis acidified with hydrochloric acid at 10° C. to 15° C.
10. 10
    استخلاصthe desired product extracted with ether
11. 11
    استخلاصThe ethereal extract
12. 12
    تجفيفis dried (Na2SO4)
13. 13
    أخرىthe ether removed
14. 14
    workup.DISTILLATIONthe residue distilled in vacuo

الإجراء التجريبي

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.

المصدر