聚[6-[4-(4-氰基苯基)苯氧基]己基甲基丙烯酸酯] → 2-乙烯基环丙烷-1,1-二甲酸二乙酯

HRID 127019

反应方程式

HRID 127019 反应方程式
[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]

参与物

6

反应物 4

HCID 962聚[6-[4-(4-氰基苯基)苯氧基]己基甲基丙烯酸酯]HCID 3283乙醚HCID 7761丙二酸二乙酯HCID 15122顺式-1,4-二氯-2-丁烯

产物 1

HCID 1110252-乙烯基环丙烷-1,1-二甲酸二乙酯

试剂、催化剂与溶剂 1

HCID 702乙醇溶剂

实验过程

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.

后处理

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

来源与证据

ORD记录
ord-f2bf6351d33642db97c4ba267c1af320
来源数据集
uspto-grants-1981_03
专利号
US04254284

关联笔记

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