反应详情

温度

70 °C

To an ice-cooled solution of 2-[(3R)-3-methoxymethylmorpholino]ethanol (505 mg) in toluene (2.5 ml) was added dropwise a solution of thionyl chloride (429 mg) in toluene (1.5 ml) below 5° C. under nitrogen atmosphere. The mixture was stirred at 70° C. for 1.5 hours. After the mixture was cooled at room temperature, ethyl acetate was added to the mixture, and resulting suspension was evaporated under reduced pressure. Diisopropyl ether was added to the residue, and after the mixture was stirred at room temperature for 15 minutes, the resulting precipitates were collected by filtration, washed with diisopropyl ether and dried at 40° C. under reduced pressure to give (3R)-4-(2-chloroethyl)-3-(methoxymethyl)morpholine hydrochloride (620 mg) as a light yellowish powder.

1. temperatureAfter the mixture was cooled at room temperature
2. customresulting suspension
3. customwas evaporated under reduced pressure
4. additionDiisopropyl ether was added to the residue
5. stirringafter the mixture was stirred at room temperature for 15 minutes
6. customthe resulting precipitates
7. filtrationwere collected by filtration
8. washwashed with diisopropyl ether
9. customdried at 40° C. under reduced pressure