Ethylene Glycol → Ethyl acetoacetate ethyleneglycol ketal

HRID 2352386ノート

反応式

HRID 2352386 の反応式
C1C=CC=CC=1.[C:7]([CH2:10][C:11]([O:13][CH2:14][CH3:15])=[O:12])(=[O:9])[CH3:8].[CH2:16](O)[CH2:17][OH:18]>C1(C)C=CC(S(O)(=O)=O)=CC=1>[CH2:16]1[CH2:17][O:18][C:7]([CH3:8])([CH2:10][C:11]([O:13][CH2:14][CH3:15])=[O:12])[O:9]1

参加物

5

反応物 3

HCID 174Ethylene GlycolHCID 241BenzeneHCID 8868Ethyl Acetoacetate

生成物 1

HCID 80865Ethyl acetoacetate ethyleneglycol ketal収率 92%

試薬・触媒・溶媒 1

HCID 6101p-Toluenesulfonic acid触媒

実験手順

Benzene (50 cc), ethyl acetylacetate (30 g, 231 mmol) and ethylene glycol (16 g), followed by p-toluenesulphonic acid (0.5 g), are introduced into a round-bottomed flask fitted with a Dean and Stark apparatus. The mixture is heated under reflux while the azeotrope is distilled off for 2 hours 30 minutes. After the removal of benzene, ethyl 3,3-ethylenedioxybutanoate (37 g) is obtained (B.P.12 =98° C.).

後処理

  1. additionare introduced into a round-bottomed flask
  2. customfitted with a Dean and Stark apparatus
  3. temperatureThe mixture is heated
  4. temperatureunder reflux while the azeotrope
  5. distillationis distilled off for 2 hours 30 minutes
  6. customAfter the removal of benzene

出典と根拠

ORDレコード
ord-0a867b0b1719436abb0488edbcac32a9
出典データセット
uspto-grants-1989_10
特許番号
US04876370

反応ノート

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