3-(benzyl(2-hydroxyethyl)amino)-2-chloro-propanenitrile

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: The crude compound 3-(benzyl(2-hydroxyethyl)amino)-2-chloro-propanenitrile 2b (8 g, 0.03 mol) was dissolved in 70 mL of tetrahydrofuran followed by the addition of potassium tert-butanolate (5.50 g, 0.05 mol) in an ice-water bath. The resulting solution was stirred for 2 hours, heated to reflux for 1 hour, added with 50 mL of saturated sodium carbonate solution, and extracted with ethyl acetate (40 mL×3). The combined organic phase was washed with saturated sodium chloride solution (50 mL×3), then dried over anhydrous magnesium sulfate, filtered and the filtrate was concentrated under reduced pressure. The resulting residue was purified by silica gel column chromatography to obtain the title compound 4-benzylmorpholine-2-carbonitrile 2c (2.71 g, yield: 41.0%) as a yellow oil liquid. heated to reflux for 1 hour extracted with ethyl acetate (40 mL×3) The combined organic phase was washed with saturated sodium chloride solution (50 mL×3) dried over anhydrous magnesium sulfate filtered the filtrate was concentrated under reduced pressure The resulting residue was purified by silica gel column chromatography

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: 2-(benzylamino)ethanol 2a (5 g, 0.03 mol) and 2-chloro-propenenitrile (3 g, 0.03 mol) were dissolved in 50 mL of anhydrous ethyl ether in an ice-water bath, heated to room temperature and stirred for 12 hours. The reaction solution was concentrated under reduced pressure to obtain the crude title compound 3-(benzyl(2-hydroxyethyl)amino)-2-chloro-propanenitrile 2b (7 g) as a red oil liquid, which was used in the next step without further furification. The reaction solution was concentrated under reduced pressure

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: 2-(benzylamino)ethanol 2a (5 g, 0.03 mol) and 2-chloro-propenenitrile (3 g, 0.03 mol) were dissolved in 50 mL of anhydrous ethyl ether in an ice-water bath, heated to room temperature and stirred for 12 hours. The reaction solution was concentrated under reduced pressure to obtain the crude title compound 3-(benzyl(2-hydroxyethyl)amino)-2-chloro-propanenitrile 2b (7 g) as a red oil liquid, which was used in the next step without further furification. The reaction solution was concentrated under reduced pressure

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: 2-(benzylamino)ethanol 2a (5 g, 0.03 mol) and 2-chloro-propenenitrile (3 g, 0.03 mol) were dissolved in 50 mL of anhydrous ethyl ether in an ice-water bath, heated to room temperature and stirred for 12 hours. The reaction solution was concentrated under reduced pressure to obtain the crude title compound 3-(benzyl(2-hydroxyethyl)amino)-2-chloro-propanenitrile 2b (7 g) as a red oil liquid, which was used in the next step without further furification. The reaction solution was concentrated under reduced pressure