二氯甲烷 → 2-Methylene-3-quinuclidone

HRID 745539

反应方程式

HRID 745539 反应方程式
Cl.O.O.[CH2:4]=[C:5]1[C:10](=[O:11])[CH:9]2[CH2:12][CH2:13][N:6]1[CH2:7][CH2:8]2.C(=O)([O-])[O-].[K+].[K+].C(Cl)Cl>O>[CH2:4]=[C:5]1[C:10](=[O:11])[CH:9]2[CH2:12][CH2:13][N:6]1[CH2:7][CH2:8]2

参与物

5

反应物 3

HCID 6344二氯甲烷HCID 11430碳酸钾HCID 219542752-Methylene-3-quinuclidinone dihydrate hydrochloride

产物 1

HCID 3229732-Methylene-3-quinuclidone

试剂、催化剂与溶剂 1

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

Suspend 95.4 g (0.455 mole) 2-methylene-3-quinuclidinone dihydrate hydrochloride in a solution of 255 g (1.85 moles) anhydrous potassium carbonate dissolved in 350 ml H2O. When the suspension clears add 500 ml methylene chloride and mix the 2-phase system overnight using a mechanical stirrer. Separate the layers and dry the methylene chloride layer over potassium carbonate. Remove the solvents in vacuo to obtain the title compound. Repeat the extraction until most of the product is collected.

后处理

  1. additionmix the 2-phase system overnight
  2. customSeparate the layers
  3. dry with materialdry the methylene chloride layer over potassium carbonate
  4. customRemove the solvents in vacuo

来源与证据

ORD记录
ord-8487bf1433834c318e8cfa3a4af4c32e
来源数据集
uspto-grants-1986_07
专利号
US04599344

关联笔记

加载中…