HRID1417824
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
A mixture of (-)-(isochroman-1-yl)acetone (LXXXIV, 0.73 g), ammonium acetate (1.48 g), methanol (2.5 ml), and THF (2.5 ml) is stirred for 25 min and then acetic acid (1.5 ml) and sodium cyanoborohydride (0.48 g) are added. After stirring for 2 hr, the mixture is concentrated and the residue is stirred with dichloromethane and sodium hydroxide (4N). The mixture is extracted with dichloromethane and washed with saline/sodium hydroxide (1N). The organic phase is separated and dried over sodium sulfate to give 2-[(-)-isochroman-1-yl]-(±)-1-methylethylamine.
WORKUP
后处理
- stirringAfter stirring for 2 hr
- concentrationthe mixture is concentrated
- stirringthe residue is stirred with dichloromethane and sodium hydroxide (4N)
- extractionThe mixture is extracted with dichloromethane
- washwashed with saline/sodium hydroxide (1N)
- customThe organic phase is separated
- dry with materialdried over sodium sulfate