HRID1605092

反应详情

EQUATION

反应方程式

HRID 1605092 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

PROCEDURE

实验过程

To a steam bath warmed mixture of 1.5 g sodium hydride in 25 ml. of dry dimethylformamide was added, dropwise and with stirring, 9.15 g. of benzyl 1,2,3,4-tetrahydrocarbazole-4-carboxylate in 25 ml. dry dimethylformamide followed by 5.4 g. of 4-toluoyl chloride in 15 ml. dry dimethylformamide, and heating was continued for two hours. The mixture was cooled and diluted with ether and 1.5 ml. glacial acetic acid. Water was added, the layers were separated and the ether extract was washed with water, 5% potassium bicarbonate solution, 1% aqueous hydrochloric acid and water, and dried over magnesium sulfate. The ether was evaporated to give the title compound which was used without purification in the next step.

WORKUP

后处理

  1. temperatureTo a steam bath warmed
  2. temperatureThe mixture was cooled
  3. customthe layers were separated
  4. extractionthe ether extract
  5. washwas washed with water, 5% potassium bicarbonate solution, 1% aqueous hydrochloric acid and water
  6. dry with materialdried over magnesium sulfate
  7. customThe ether was evaporated