HRID240309
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- extractionextracted with CH2Cl2 (2×5 ml)
- dry with materialOrganic phase was dried over Na2SO4
- filtrationfiltered
- customevaporated
- dissolutionThe residue was dissolved in THF (2 ml)
- customThe solvent was evaporated
- washthe crude solid washed with EtOH
- customdried under vacuum