海萝胶 → 2-Ethyl-2-methyl-indan

HRID 261529

反应方程式

HRID 261529 反应方程式
Cl.[CH2:2]([C:4]1([CH3:14])[CH2:12][C:11]2[C:6](=[CH:7][CH:8]=[CH:9][CH:10]=2)[C:5]1=O)[CH3:3]>O.C(O)C.[Zn].C([O-])(=O)C.[Hg+2].C([O-])(=O)C>[CH2:2]([C:4]1([CH3:14])[CH2:12][C:11]2[C:6](=[CH:7][CH:8]=[CH:9][CH:10]=2)[CH2:5]1)[CH3:3]

参与物

7

反应物 2

HCID 313海萝胶HCID 146860942-Ethyl-2-methyl-1-indanone

产物 1

HCID 203944402-Ethyl-2-methyl-indan

试剂、催化剂与溶剂 4

HCID 15337乙酸汞催化剂HCID 23994Zinc催化剂HCID 702乙醇溶剂HCID 962聚[6-[4-(4-氰基苯基)苯氧基]己基甲基丙烯酸酯]溶剂

实验过程

335 g of zinc dust and 33.5 g of mercury (II) acetate and a solution of 330 cc of concentrated hydrochloric acid in 280 cc of water are rapidly added dropwise in a stirring apparatus. The mixture is boiled at reflux and a solution of 63 g of 2-ethyl-2-methyl-1-indanone in 525 cc of ethanol is added dropwise within 10 minutes while stirring. The reaction mixture is subsequently stirred at reflux for 28 hours, cooled, filtered, and the residue is washed with water/petroleum ether. The filtrate is extracted with petroleum ether, the petroleum ether extract is washed with water and dried over sodium sulphate. The crude 2-ethyl-2-methyl-indan, obtained as an oil after evaporating the solvent, is purified by chromatography on aluminium oxide/petroleum ether.

后处理

  1. temperatureat reflux
  2. stirringThe reaction mixture is subsequently stirred
  3. temperatureat reflux for 28 hours
  4. temperaturecooled
  5. filtrationfiltered
  6. washthe residue is washed with water/petroleum ether
  7. extractionThe filtrate is extracted with petroleum ether
  8. extractionthe petroleum ether extract
  9. washis washed with water
  10. dry with materialdried over sodium sulphate

来源与证据

ORD记录
ord-28adf486cf104b4d8d97dd240ed54f30
来源数据集
uspto-grants-1979_08
专利号
US04166131

关联笔记

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