反应详情

In 40 ml of methanol under cooling 11.5 ml (0.215 mol) of 100% sulfuric acid is dissolved, the solution is heated under reflux conditions for 30 minutes, then after cooling, to room temperature 12.4 g (0.042 mol) of dextrorotatory [2-(2-thienyl)ehylamino](2-chlorophenyl)acetamide is added and the mixture is heated under reflux for 6-7 hours, till the end of the reaction. Methanol is distilled off in vacuo, to the residue 75 ml of 1,2-dichloroethane and 75 ml of water are added, the mixture is shaken well and the phases are separated. The aqueous phase is extracted with 2×20 ml of 1,2-dichloroethane, the unified organic phase is extracted with 50 ml of 5% sodium hydroxide solution then with 50 ml of water, dried over anhydrous sodium sulfate. The drying material is filtered off and 1.5 g (0.041 mol) of dry hydrogen chloride gas is introduced under cooling into the solution. The precipitated crystalline product is filtered off, washed with 1,2-dichloroethane and dried. Weight: 12.1 g, mp.: 185-186° C. (decomposition), [α]22D=+107°. Yield: 83%. Optical purity: in general 99-100%.

1. dissolutionis dissolved
2. temperaturethe solution is heated under reflux conditions for 30 minutes
3. additionis added
4. temperaturethe mixture is heated
5. temperatureunder reflux for 6-7 hours, till the end of the reaction
6. distillationMethanol is distilled off in vacuo, to the residue 75 ml of 1,2-dichloroethane and 75 ml of water
7. additionare added
8. customthe phases are separated
9. extractionThe aqueous phase is extracted with 2×20 ml of 1,2-dichloroethane
10. extractionthe unified organic phase is extracted with 50 ml of 5% sodium hydroxide solution
11. dry with materialwith 50 ml of water, dried over anhydrous sodium sulfate
12. filtrationThe drying material is filtered off
13. temperatureunder cooling into the solution
14. filtrationThe precipitated crystalline product is filtered off
15. washwashed with 1,2-dichloroethane
16. customdried