反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
产物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
(4-Benzylmorpholin-2-yl)methanamine 2d (1.35 g, 6.50 mmol) was dissolved in 30 mL of ethanol followed by the addition of L-(−)-dibenzoyltartaric acid (2.34 g, 6.50 mmol). The reaction solution was heated to reflux for 10 minutes, then cooled down to room temperature, placed for 16 hours resulting in the formation of crystal and filtered. The filter cake was dissolved in 10 mL of water, added with 1 M aqueous sodium hydroxide solution to adjust pH to 9 and extracted with dichloromethane (30 mL×3). The combined organic phase was dried over anhydrous sodium sulfate, filtered and the filtrate was concentrated under reduced pressure to obtain the title compound [(2R)-4-benzylmorpholin-2-yl]methanamine 15a (0.28 g, yield: 28.0%) as a light yellow oil liquid.
WORKUP
后处理
- temperatureThe reaction solution was heated
- temperatureto reflux for 10 minutes
- customresulting in the formation of crystal
- filtrationfiltered
- dissolutionThe filter cake was dissolved in 10 mL of water
- additionadded with 1 M aqueous sodium hydroxide solution
- extractionextracted with dichloromethane (30 mL×3)
- dry with materialThe combined organic phase was dried over anhydrous sodium sulfate
- filtrationfiltered
- concentrationthe filtrate was concentrated under reduced pressure