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
In this reference example, 9.76 g of salicylaldehyde, 15.12 g of 1-benzyl-4-amino-piperidine and 100 ml of methanol are mixed and stirred at room temperature for one hour. While the resultant mixture is cooled with ice, 3.2 g of sodium borohydride is added thereto over a period of one hour and 30 minutes. Then, the mixture is stirred at room temperature for 2 hours. The resultant reaction mixture is poured into 1 l of ice water. The light yellow crystals deposited are separated by filtration and then dissolved in 200 ml of ethyl acetate. The ethyl acetate solution is washed with a saturated aqueous sodium chloride, dried and subsequently concentrated under reduced pressure to obtain 19.0 g of light yellow crystals. The crystals are recrystallized from ethanol to obtain 12.0 g of the desired product.
WORKUP
后处理
- additionis added
- waitover a period of one hour
- custom30 minutes
- stirringThen, the mixture is stirred at room temperature for 2 hours
- customThe resultant reaction mixture
- customThe light yellow crystals deposited are separated by filtration
- dissolutiondissolved in 200 ml of ethyl acetate
- washThe ethyl acetate solution is washed with a saturated aqueous sodium chloride
- customdried
- concentrationsubsequently concentrated under reduced pressure