2,3-Dimethyl-2-butene → Ethyl 2,2,3,3-tetramethylcyclopropane-carboxylate

HRID 462858ノート

反応式

HRID 462858 の反応式
[CH3:1][C:2](=[C:4]([CH3:6])[CH3:5])[CH3:3].[N+](=[CH:9][C:10]([O:12][CH2:13][CH3:14])=[O:11])=[N-]>>[CH3:1][C:2]1([CH3:3])[C:4]([CH3:6])([CH3:5])[CH:9]1[C:10]([O:12][CH2:13][CH3:14])=[O:11]

参加物

3

反応物 2

HCID 112502,3-Dimethyl-2-butene2 回HCID 12192Ethyl diazoacetate

生成物 1

HCID 136614Ethyl 2,2,3,3-tetramethylcyclopropane-carboxylate

実験手順

The method of Mesheheryakov, Chem. Abstr., 54, 24436d (1960) was employed. To a mixture of 19 g. (0.226 mole) of 2,3-dimethyl-2-butene and 2 g. of cupric sulfate is added at reflux a mixture of 51 g. (0.447 mole) ethyl diazoacetate and 19 g. of 2,3-dimethyl-2-butene. The resulting mixture is heated at reflux for 3 hours, cooled, filtered and distilled to afford 19.8 g. (26%) of the desired cyclic ester, B.P. 76°-77° (15 mm.).

後処理

  1. additionTo a mixture of 19 g
  2. temperatureat reflux
  3. additiona mixture of 51 g
  4. temperatureThe resulting mixture is heated
  5. temperatureat reflux for 3 hours
  6. temperaturecooled
  7. filtrationfiltered
  8. distillationdistilled
  9. customto afford 19.8 g

出典と根拠

ORDレコード
ord-dc58bb1051964ce99de7e47a877ccbdf
出典データセット
uspto-grants-1985_05
特許番号
US04517379

反応ノート

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