HRID346083
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
To a stirred mixture of 24 parts of indoline and 83 parts of powdered anhydrous potassium carbonate in 150 parts of acetonitrile was added 50 parts of 2-bromoethanol. The mixture was gradually warmed to reflux and kept at reflux temperature for 8 hours. The mixture was filtered and the solvent was removed. The product was purified by column chromatography on a silica gel column. The eluents were 1:1 mixture of hexane with methylene chloride and then ethyl acetate. The product was 29 parts with a boiling point of 118° C. at 0.5 torr. Proton and carbon-13 NMR spectra were consistent with structure.
WORKUP
后处理
- temperatureThe mixture was gradually warmed
- temperatureto reflux
- temperatureat reflux temperature for 8 hours
- filtrationThe mixture was filtered
- customthe solvent was removed
- customThe product was purified by column chromatography on a silica gel column
- addition1:1 mixture of hexane with methylene chloride