反应详情

温度

120 °C

1-(phenylmethyl)-4-[1-(phenylmethyl)-1H-imidazol-2-yl]-4-piperidinol (0.124 mol) and AlCl3 (0.31 mol) were stirred in a melt at 120° C. for 1 h. The mixture was cooled, AlCl3 (0.31 mol) was added and the mixture was stirred at 120° C. for 1 h. The mixture was poured into ice, alkalized with NaOH 50% and extracted with CH2Cl2. The organic layer was dried (MgSO4), filtered off and evaporated. The residue was purified by HPLC (eluent: CH2Cl2/(CH3OH/NH3) 99/1). The pure fractions were collected and evaporated. The residue was converted into the hydrochloric acid salt (1:2) in (C2H5)2O, yielding 0.91 g of 1′-(phenylmethyl)spiro[imidazo[1,2-b]isoquinoline-10[5H],4′-piperidine]dihydrochloride.dihydrate (2%) (interm. 3; mp. 161.2° C.).

1. temperatureThe mixture was cooled
2. additionThe mixture was poured into ice
3. extractionextracted with CH2Cl2
4. dry with materialThe organic layer was dried (MgSO4)
5. filtrationfiltered off
6. customevaporated
7. customThe residue was purified by HPLC (eluent: CH2Cl2/(CH3OH/NH3) 99/1)
8. customThe pure fractions were collected
9. customevaporated