HRID2372335

反应详情

EQUATION

反应方程式

HRID 2372335 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Into a suspension of 0.95 g of lithium aluminum hydride and 100 ml of tetrahydrofuran, a solution obtained by dissolving 1.77 g of 4-dimethylaminocarbonylbenzylamine prepared in Reference Example 5 in 50 ml of tetrahydrofuran, was dropwise added under stirring, and the reaction solution was refluxed for 3 hours. After cooling, the reaction solution was cooled with ice, and ice pieces were gradually added to decompose the excessive reducing agent. Tetrahydrofuran was distilled off, and the residue thereby obtained was extracted with dichloromethane. The extract was washed with water and a saturated sodium chloride aqueous solution, and dried over sodium sulfate, and then the solvent was distilled off to obtain 1.13 g of the above identified compound as a pale yellow oily substance.

WORKUP

后处理

  1. customa solution obtained
  2. additionwas dropwise added
  3. temperaturethe reaction solution was refluxed for 3 hours
  4. temperatureAfter cooling
  5. temperaturethe reaction solution was cooled with ice, and ice pieces
  6. additionwere gradually added
  7. distillationTetrahydrofuran was distilled off
  8. customthe residue thereby obtained
  9. extractionwas extracted with dichloromethane
  10. washThe extract was washed with water
  11. dry with materiala saturated sodium chloride aqueous solution, and dried over sodium sulfate
  12. distillationthe solvent was distilled off
  13. customto obtain 1.13 g of the