HRID346083

反应详情

EQUATION

反应方程式

HRID 346083 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

  1. temperatureThe mixture was gradually warmed
  2. temperatureto reflux
  3. temperatureat reflux temperature for 8 hours
  4. filtrationThe mixture was filtered
  5. customthe solvent was removed
  6. customThe product was purified by column chromatography on a silica gel column
  7. addition1:1 mixture of hexane with methylene chloride