反应详情

温度

27.5 °C

Added 50 liters of 20% sodium hydroxide solution to a cooled solution of 100 Kgs. of 3-(dimethylamino)-1-(thiophen-2-yl) propan-1-one hydrochloride, 100 liters of methanol and 25 liters of water at 0-5° C. Added a solution of 10 Kgs. of sodium borohydride in 50 liters of 20% sodium hydroxide to the above reaction mixture slowly at 0-5° C. in 5 hours. Allowed the reaction mixture temperature to 25-30° C. Stirred the reaction mixture for 6 hours at 25-30° C. Extracted the reaction mixture with methylene chloride. Separated the organic and aqueous layers. Extracted the aqueous layer with methylene chloride. Washed the organic layer with 10% sodium chloride solution. Distilled the solvent completely under reduced pressure at below 40° C. Added 25 liters of hexanes to the above reaction mixture. Distilled the solvent completely under reduced pressure at below 40° C. Added 100 liters of hexanes to the above reaction mixture. Heated the reaction mixture to reflux. Stirred the reaction mixture for 60 minutes. Cooled the reaction mixture to 0-5° C. and stirred the reaction mixture for 3 hours. Filtered the precipitated solid and washed with chilled hexanes. Dried the material at 50-55° C. for 6 hours to get the title compound.

1. customat 0-5° C
2. customto 25-30° C
3. extractionExtracted the reaction mixture with methylene chloride
4. customSeparated the organic and aqueous layers
5. extractionExtracted the aqueous layer with methylene chloride
6. washWashed the organic layer with 10% sodium chloride solution
7. distillationDistilled the solvent completely under reduced pressure at below 40° C
8. additionAdded 25 liters of hexanes to the above reaction mixture
9. distillationDistilled the solvent completely under reduced pressure at below 40° C
10. additionAdded 100 liters of hexanes to the above reaction mixture
11. temperatureHeated the reaction mixture
12. temperatureto reflux
13. stirringStirred the reaction mixture for 60 minutes
14. temperatureCooled the reaction mixture to 0-5° C.
15. stirringstirred the reaction mixture for 3 hours
16. filtrationFiltered the precipitated solid
17. washwashed with chilled hexanes
18. customDried the material at 50-55° C. for 6 hours