Methyl Acetate → Methyl 4,4-diethoxy-3-oxobutanoate

HRID 1607724

反応式

HRID 1607724 の反応式
C(O[C:4](=[O:12])[CH:5]([O:9][CH2:10][CH3:11])[O:6][CH2:7][CH3:8])C.[CH3:13][O:14][C:15](=[O:17])[CH3:16].[Na]>>[CH2:10]([O:9][CH:5]([O:6][CH2:7][CH3:8])[C:4](=[O:12])[CH2:16][C:15]([O:14][CH3:13])=[O:17])[CH3:11]

参加物

4

反応物 3

HCID 6584Methyl Acetate2 回HCID 80169Ethyl diethoxyacetateHCID 5360545Sodium3 回

生成物 1

HCID 15445487Methyl 4,4-diethoxy-3-oxobutanoate

実験手順

Ethyldiethoxyacetate (32 g.) and methylacetate (25 g.) are placed in a flask equipped with stirred 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.

後処理

  1. customequipped
  2. temperaturereflux condenser
  3. temperatureheated to reflux
  4. temperatureheating
  5. dissolutionis completely dissolved
  6. temperatureheating
  7. temperatureThe mixture is cooled
  8. extractionthe mixture extracted with ether
  9. customis acidified with hydrochloric acid at 10° C. to 15° C.
  10. extractionthe desired product extracted with ether
  11. extractionThe ethereal extract
  12. dry with materialis dried (Na2SO4)
  13. customthe ether removed
  14. distillationthe residue distilled in vacuo

出典と根拠

ORDレコード
ord-6d8546fa883841339191ad0839d981db
出典データセット
uspto-grants-1989_09
特許番号
US04866175

関連ノート

読み込み中…