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

HRID 127019

반응식

HRID 127019 반응식
[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]

참가 물질

6

반응물 4

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

생성물 1

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

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

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.

후처리

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

출처 및 근거

ORD 기록
ord-f2bf6351d33642db97c4ba267c1af320
출처 데이터셋
uspto-grants-1981_03
특허 번호
US04254284

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