Water → Diethyl 2-vinylcyclopropane-1,1-dicarboxylate

HRID 225015

反応式

HRID 225015 の反応式
[C:1]([O:9][CH2:10][CH3:11])(=[O:8])[CH2:2][C:3]([O:5][CH2:6][CH3:7])=[O:4].Cl[CH2:13][CH:14]=[CH:15][CH2:16]Cl.O.CCOCC>C(O)C>[CH2:10]([O:9][C:1]([C:2]1([C:3]([O:5][CH2:6][CH3:7])=[O:4])[CH2:16][CH:15]1[CH:14]=[CH2:13])=[O:8])[CH3:11]

参加物

6

反応物 4

HCID 962WaterHCID 3283Diethyl EtherHCID 7761Diethyl MalonateHCID 151221,4-Dichloro-2-butene

生成物 1

HCID 111025Diethyl 2-vinylcyclopropane-1,1-dicarboxylate

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

To a solution of 18.4 g (2 equivalents) in 300 ml of anhydrous ethanol is added rapidly 164 g (1 equivalent) of diethyl malonate. 1,4-Dichloro-2-butene (98% mixture of cis and trans, Aldrich) (50 g, 1 equivalent) is slowly added to the warm, stirred suspension of the diethyl sodio malonate during 15 minutes after which the mixture is refluxed for 3 hours. Upon cooling, the mixture is poured into 1.2 liters of water and an oil isolated by ether extraction. The ether extract is dried over magnesium sulfate and distilled to give 1,1-bis-ethoxycarbonyl-2-vinylcyclopropane, B.P. 108°-116° C./14 mm.

後処理

  1. temperatureis refluxed for 3 hours
  2. temperatureUpon cooling
  3. extractionThe ether extract
  4. dry with materialis dried over magnesium sulfate
  5. distillationdistilled

出典と根拠

ORDレコード
ord-480bacf56dde4444839f59b523999428
出典データセット
uspto-grants-1980_11
特許番号
US04235778

関連ノート

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