反应详情

3-[3-(Methoxymethoxy)-1-(2-thienyl)cyclobutyl]-5,6,7,8,9,10-hexahydro[1,2,4]triazolo[4,3-a]azocine (6.14 g) was dissolved in methylene chloride (125 ml) and then trifluoroacetic acid (25 ml) was added thereto, followed by stirring at room temperature for 21 hours. The reaction solution was subjected to evaporation under reduced pressure and the resulting residue was diluted with a 1M aqueous sodium hydroxide solution (100 ml), followed by extraction with chloroform (100 ml×2). The organic layer was dried over anhydrous sodium sulfate, and filtered and then the solvent was removed by evaporation under reduced pressure. The resulting solid washed with diethyl ether to obtain 3.84 g of 3-(5,6,7,8,9,10-hexahydro[1,2,4]triazolo[4,3-a]azocin-3-yl)-3-(2-thienyl)cyclobutanol (white solid).

1. customThe reaction solution was subjected to evaporation under reduced pressure
2. additionthe resulting residue was diluted with a 1M aqueous sodium hydroxide solution (100 ml)
3. extractionfollowed by extraction with chloroform (100 ml×2)
4. dry with materialThe organic layer was dried over anhydrous sodium sulfate
5. filtrationfiltered
6. customthe solvent was removed by evaporation under reduced pressure
7. washThe resulting solid washed with diethyl ether