反应详情

12.5 g (26 mmol) of 1-(4-benzyloxyphenyl)-2-(4-diphenylmethyl-piperazinyl)ethanone and 2.8 g (26 mmol) of anisole were dissolved in a mixture of 37.5 ml of acetic acid and 12.5 ml of 47% hydrobromic acid. The resultant mixture was heated to reflux for 1 hour. After being cooled to room temperautre, the reaction mixture was washed with 200 ml of ether and then with 50 ml of ether to remove acetic acid. The resultant solution was neutralized with an aqueous 2N solution of sodium hydroxide. Separated organic substances were extracted with 120 ml of ethyl acetate and then washed with saturated saline. The ethyl acetate solution was dried over anhydrous sodium sulfate and then concentrated. The residue was taken up in 60 ml of isopropanol and allowed to stand at room temperature to give 6.28 g of crude crystals of 2-(4-diphenylmethylpiperazinyl)-1-(4-hydroxyphenyl)ethanone (yield: 62%).

1. temperatureto reflux for 1 hour
2. temperatureAfter being cooled to room temperautre
3. washthe reaction mixture was washed with 200 ml of ether
4. customwith 50 ml of ether to remove acetic acid
5. extractionSeparated organic substances were extracted with 120 ml of ethyl acetate
6. washwashed with saturated saline
7. dry with materialThe ethyl acetate solution was dried over anhydrous sodium sulfate
8. concentrationconcentrated
9. customto stand at room temperature