反応 #45297

反応方程式

water

water

t-Butylamine

m-chloro-α-bromopropiophenone

t-butylamine

→

bupropion hydrochloride

溶媒

acetone

Acetone

反応条件

後処理

1. 1
   温度the reaction mixture was refluxed for 2.5 hours
2. 2
   その他was evaproated at the temperature of 120° C
3. 3
   抽出extracted with 1500 ml of chloroform and 250 ml of water
4. 4
   乾燥The organic phase was dried with anhydrous sodium sulfate (30 g)
5. 5
   濃縮concentrated to dryness under reduced pressure
6. 6
   workup.ADDITIONA solution of HCl in ethanol was added to the concentrated solution at room temperature

実験手順

t-Butylamine was added to a solution of m-chloro-α-bromopropiophenone obtained above in acetone and water and the reaction mixture was refluxed for 2.5 hours. Acetone, water and excessive t-butylamine was evaproated at the temperature of 120° C. The concentrated solution was cooled down to room temperature and then extracted with 1500 ml of chloroform and 250 ml of water. The organic phase was dried with anhydrous sodium sulfate (30 g) and concentrated to dryness under reduced pressure. A solution of HCl in ethanol was added to the concentrated solution at room temperature and a crude product of bupropion hydrochloride was obtained after filtration. The crude product of bupropion hydrochloride was added to 2000 ml ethanol and heated to 70° C., decolorized by activated carbon (2 g) for 30 minutes and filtered. The filtrate was cooled and filtered to obtain wet product of bupropion hydrochloride. The wet product was dried in vacuum (−0.04˜−0.09 MPa, 70° C.) for 4 hours to obtain pure product. Total yield was 72% based on m-chloropropiophenone; and the HPLC's purify was ≧99.9%.

出典