反応 #45295

反応方程式

t-Butylamine

m-chloro-α-bromopropiophenone

→

bupropion

反応条件

後処理

1. 1
   その他obtained above and the reaction mixture
2. 2
   温度was refluxed for 3 hours
3. 3
   その他Excessive t-butylamine was removed by evaporation below 80° C
4. 4
   抽出extracted with 800 ml of ethyl acetate and 280 ml of water
5. 5
   乾燥The organic phase was dried with anhydrous magnesium sulfate (15 g)

実験手順

t-Butylamine was added to m-chloro-α-bromopropiophenone obtained above and the reaction mixture was refluxed for 3 hours. Excessive t-butylamine was removed by evaporation below 80° C. The concentrated solution was cooled down to room temperature and then extracted with 800 ml of ethyl acetate and 280 ml of water. The organic phase was dried with anhydrous magnesium sulfate (15 g) to obtain a solution of bupropion free base. A solution of HCl in ethyl acetate was added at room temperature to the organic phase. Crude product of bupropion hydrochloride was obtained after filtration. The crude product of bupropion hydrochloride was dissolved in 1200 ml of methanol and 120 ml of water at 80° C., decolorized with activated carbon (5 g) for 20 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, 80° C.) for 3 hours to obtain pure product. Total yield was 70% based on m-chloropropiophenone, and the HPLC's purify was higher than or equal to 99.9%.

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