HRID2364697

反应详情

EQUATION

反应方程式

HRID 2364697 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

  1. temperatureThe reaction solution was heated
  2. temperatureto reflux for 10 minutes
  3. customresulting in the formation of crystal
  4. filtrationfiltered
  5. dissolutionThe filter cake was dissolved in 10 mL of water
  6. additionadded with 1 M aqueous sodium hydroxide solution
  7. extractionextracted with dichloromethane (30 mL×3)
  8. dry with materialThe combined organic phase was dried over anhydrous sodium sulfate
  9. filtrationfiltered
  10. concentrationthe filtrate was concentrated under reduced pressure