HRID240309

反应详情

EQUATION

反应方程式

HRID 240309 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

4,4-Difluoropiperidine hydrochloride (249 mg, 1.58 mmol) was dissolved in 1N NaOH (5 ml) and extracted with CH2Cl2 (2×5 ml). Organic phase was dried over Na2SO4, filtered and evaporated. The residue was dissolved in THF (2 ml) and this solution was added to a solution of 1 (185 mg, 0.79 mmol) in THF (2 ml); the mixture was stirred at room temperature for 48 hours. The solvent was evaporated, the crude solid washed with EtOH and dried under vacuum, affording 8 (245 mg, 95%) as yellow-brown solid.

WORKUP

后处理

  1. extractionextracted with CH2Cl2 (2×5 ml)
  2. dry with materialOrganic phase was dried over Na2SO4
  3. filtrationfiltered
  4. customevaporated
  5. dissolutionThe residue was dissolved in THF (2 ml)
  6. customThe solvent was evaporated
  7. washthe crude solid washed with EtOH
  8. customdried under vacuum