反应详情

A mixture of 4.5 g of 1,3-bis[4-(4-methoxybenzyl)-1-piperazinyl]propane from Example 19 and 125 ml of 49% hydrobromic acid was refluxed for 2 hours and was then cooled and diluted with 125 ml of water. After filtration the aqueous solution was neutralized with 2N sodium hydroxide to adjust the pH to 8. The resulting mixture was extracted three times each with 150 ml of ethanol. The alcohol was then removed by rotary evaporation and the residue was chromatographed on silica with the eluant being methylene chloride containing 1% ammonium hydroxide and 10% methanol to obtain 1.3 g (31% of theory) of 1,3-bis[4-(4-hydroxybenzyl)-1-piperazinyl]propane as a white crystalline product, melting at 197°-201° C.

1. temperaturewas refluxed for 2 hours
2. temperaturewas then cooled
3. filtrationAfter filtration the aqueous solution
4. extractionThe resulting mixture was extracted three times each with 150 ml of ethanol
5. customThe alcohol was then removed by rotary evaporation
6. customthe residue was chromatographed on silica with the eluant