反応 #73581

反応方程式

metformin hydrochloride

sodium hydroxide

→

metformin

収率 76.9%

溶媒

ethanol

反応条件

後処理

1. 1
   ろ過was filtered
2. 2
   濃縮the filtrate was concentrated under reduced pressure
3. 3
   workup.ADDITIONThen 300 Ml of acetone was added to the resulting solid
4. 4
   ろ過Insoluble material was filtered
5. 5
   濃縮the filtrate was concentrated under reduced pressure

実験手順

20.00 g (1 equivalent) of metformin hydrochloride and 4.84 g (1 equivalent) of sodium hydroxide were stirred in 200 Ml of ethanol for 2 hours at room temperature, and then remaining solid was filtered and the filtrate was concentrated under reduced pressure. Then 300 Ml of acetone was added to the resulting solid and stirred. Insoluble material was filtered, and the filtrate was concentrated under reduced pressure to obtain 12.0 g of metformin free base. 500 Ml of acetone and 10 Ml (1.45 equivalents) of glacial acetic acid were added to the metformin free base, and then the mixture was stirred. The resulting crystal was filtered and washed with acetone, and then dried at 60° C. to obtain 13.6 g of metformin acetate (yield: 59.5%).

出典