反应详情

温度

2.5 °C

A mixture of 62 Kgs. of mandelate salt of (S)-3-(dimethylamino)-1-(thiophen-2-yl) propan-1-ol, 125 liters of water and 375 liters of methylene chloride is cooled to 0-5° C. Adjusted the pH of the reaction mixture to 9.8 with 10% sodium carbonate solution at 0-5° C. Stirred the reaction mixture for 20 minutes at 0-5° C. Separated the organic and aqueous layers. Extracted the aqueous layer with methylene chloride. Washed the organic layer twice with 10% sodium chloride solution. Distilled the solvent completely under reduced pressure at below 35° C. Added 19 liters of cyclohexane to the above reaction mixture. Distilled the solvent completely under reduced pressure at below 35° C. Added 125 liters of cyclohexane to the above reaction mixture. Heated the reaction mixture to 40-45° C. and stirred for 60 minutes. Cooled the reaction mixture to 0-5° C. Filtered the precipitated solid and washed with cyclohexane. Dried the material at 40-45° C. for 6 hours to get the title compound.

1. customat 0-5° C
2. customSeparated the organic and aqueous layers
3. extractionExtracted the aqueous layer with methylene chloride
4. washWashed the organic layer twice with 10% sodium chloride solution
5. distillationDistilled the solvent completely under reduced pressure at below 35° C
6. additionAdded 19 liters of cyclohexane to the above reaction mixture
7. distillationDistilled the solvent completely under reduced pressure at below 35° C
8. additionAdded 125 liters of cyclohexane to the above reaction mixture
9. temperatureHeated the reaction mixture to 40-45° C.
10. stirringstirred for 60 minutes
11. temperatureCooled the reaction mixture to 0-5° C
12. filtrationFiltered the precipitated solid
13. washwashed with cyclohexane
14. customDried the material at 40-45° C. for 6 hours