反应详情

温度

20 °C

Accordingly the compound (2S,3R)-1-(dimethylamino)-3-(3-methoxyphenyl)-2-methyl pentan-3-ol of Formula-V was charged in the solvent tetrahydrofuran and under stirring charged concentrated sulfuric acid at temperature of 20-30° C. The reaction mixture is stirred and charged methanesulfonic acid or para toluenesulfonic acid and solvent cyclohexane. Stirred and raised the temperature to reflux. Maintained the reaction mass at reflux temperature for 3-5 hours with simultaneous removal of water. Cooled the reaction mass to 20° C. and separated the organic layer. Charged the organic layer in an autoclave and diluted the layer with tetrahydrofuran. Charged the catalyst Pd/C. Purged the autoclave with nitrogen gas and followed with hydrogen gas pressure of 5-7 kg. Maintained the reaction mass at 25-30° C. for 2-4 hours. After completion of the reaction the reaction mass was filtered and the filtrate was concentrated under reduced pressure to get the residual mass. Diluted the residual mass with water and extracted with toluene. Separated the aqueous layer and adjusted the pH to 9-10 with aqueous solution of sodium hydroxide. Extracted the aqueous layer with diisopropyl ether, separated the organic layer and concentrated under reduced pressure below 40° C. to get the compound (2R,3R)-3-(3-methoxyphenyl)-N,N,2-trimethylpentan-1-amine of Formula-VII.

1. stirringThe reaction mixture is stirred
2. stirringStirred
3. temperatureraised the temperature
4. temperatureto reflux
5. temperatureMaintained the reaction mass
6. temperatureat reflux temperature for 3-5 hours
7. customwith simultaneous removal of water
8. customseparated the organic layer
9. additionCharged the organic layer in an autoclave
10. additiondiluted the layer with tetrahydrofuran
11. additionCharged the catalyst Pd/C
12. customPurged the autoclave with nitrogen gas
13. temperatureMaintained the reaction mass at 25-30° C. for 2-4 hours
14. customAfter completion of the reaction the reaction mass
15. filtrationwas filtered
16. concentrationthe filtrate was concentrated under reduced pressure
17. customto get the residual mass
18. extractionextracted with toluene
19. customSeparated the aqueous layer
20. extractionExtracted the aqueous layer with diisopropyl ether
21. customseparated the organic layer
22. concentrationconcentrated under reduced pressure below 40° C.