反应详情

温度

71.5 °C

In a dry flask charged magnesium turning (41.0 gm 1.70 M) in tetrahydrofuran (200 ml). Under nitrogen atmosphere charged 3-Bromo anisole (20.0 gm; 0.106 M), iodine crystal (0.2 gm). Stirred and heated the reaction mass to 68-75° C. After initiation of the reaction the remaining quantity of 3-Bromo anisole (307 gm, 1.641 M) was added maintaining the reaction at reflux. Stirred and maintained the reaction mass at refluxed for 1 hrs, cooled to 25-30° C. Slowly added (2S)-1-(dimethylamino)-2-methylpentan-3-one (100.0 gm, 0.699 M) maintaining the temperature of the reaction at 25-30° C. The reaction mass was maintained for 12 hour at 25-30° C. and then quenched the reaction mass in ice cold D. M. water (1.0 Liter). Stirred and adjusted the pH of the reaction mass to 3-4 with acetic acid. Further adjusted the pH to 9-10 using ammonia solution. Stirred the reaction mass 30 minutes and extracted the reaction solution with diisopropyl ether. Combined diisopropyl ether was dried over anhydrous sodium sulphate and concentrated under reduced pressure below 40° C. to get the compound (2S,3R)-1-(dimethylamino)-3-(3-methoxyphenyl)-2-methylpentan-3-ol.

1. additionwas added
2. temperaturemaintaining
3. customthe reaction
4. temperatureat reflux
5. stirringStirred
6. temperaturemaintained the reaction mass
7. temperatureat refluxed for 1 hrs
8. temperaturecooled to 25-30° C
9. customthe temperature of the reaction at 25-30° C
10. temperatureThe reaction mass was maintained for 12 hour at 25-30° C.
11. customquenched the reaction mass in ice cold D
12. stirringStirred
13. stirringStirred the reaction mass 30 minutes
14. extractionextracted the reaction solution with diisopropyl ether
15. dry with materialCombined diisopropyl ether was dried over anhydrous sodium sulphate
16. concentrationconcentrated under reduced pressure below 40° C.