HRID542442
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
CONDITIONS
反应条件
- 温度
- 5 °C
PROCEDURE
实验过程
To a solution of 73.7 g of 3-benzylamino quinuclidine in water (≃300 to 400 ml) are added, while cooling to 5° C., 51 ml of a 40% aqueous formaldehyde solution. Then after the addition, the mixture is left for 30 minutes at 5° C., then 32 g of sodium cyanoborohydride are added within 1 to 2 hours. Then it is left at room temperature for 12 hours, extracted with ethyl acetate, the mixture obtained is dried on sodium (or magnesium) sulfate, filtered, the filtrate is evaporated and the residue is distilled (Boiling point [0.04 mm/Hg]=125° C.). Thus the expected product is obtained practically quantitatively.
WORKUP
后处理
- additionThen after the addition
- waitThen it is left at room temperature for 12 hours
- extractionextracted with ethyl acetate
- customthe mixture obtained
- dry with materialis dried on sodium (or magnesium) sulfate
- filtrationfiltered
- customthe filtrate is evaporated
- distillationthe residue is distilled (Boiling point [0.04 mm/Hg]=125° C.)