HRID51310

反应详情

EQUATION

反应方程式

HRID 51310 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A mixture of 430 mg. of the product from Example 3 Part D, 2.0 gm. of 5% Pd/C, and 20 mL of carbitol was heated to reflux and refluxed for 21 hours, cooled, and filtered. The filtrate was diluted with water, acidified with hydrochloric acid, and extracted well with ethyl acetate. The organic phase was washed with brine, dried over sodium sulfate and evaporated in vacuo. The residue was triturated with dichloromethane and filtered to remove solid tetrahydrocarbazole. The filtrate was evaporated in vacuo to give the title product, 125 mg, 31%.

WORKUP

后处理

  1. additionA mixture of 430 mg
  2. temperatureto reflux
  3. temperaturerefluxed for 21 hours
  4. temperaturecooled
  5. filtrationfiltered
  6. additionThe filtrate was diluted with water
  7. extractionextracted well with ethyl acetate
  8. washThe organic phase was washed with brine
  9. dry with materialdried over sodium sulfate
  10. customevaporated in vacuo
  11. customThe residue was triturated with dichloromethane
  12. filtrationfiltered
  13. customto remove solid tetrahydrocarbazole
  14. customThe filtrate was evaporated in vacuo