反应详情

Dissolve 3-[4-bromo-2-(2-methyl-2H-[1,2,4]triazol-3-yl)-thiazol-5-yl]-2,5-dimethyl-7-(1-propyl-butyl)-pyrazolo[1,5-a]pyrimidine (750 mg, 1.54 mmol) in acetone (5 mL) and add 1 M HCl in diethyl ether (1.84 mL, 1.84 mmol). Stir the mixture at room temperature for 3 h and concentrate in vacuo. Dissolve the residue in diethyl ether/hexane=1/1 (5 mL) and crystallize the desired HCl salt (526 mg, 65%). ES/MS m/z (81Br) 490 (M+1)+; 1H-NMR(CDCl3): 8.20 (s, 1H), 6.82 (s, 1H), 4.21 (s, 3H), 3.64 (m, 1H), 2.49 (m, 3H), 2.44 (s, 3H), 1.75 (m, 4H), 1.96(m, 4H), 0.81 (m, 6H).

1. concentrationconcentrate in vacuo
2. dissolutionDissolve the residue in diethyl ether/hexane=1/1 (5 mL)
3. customcrystallize the desired HCl salt (526 mg, 65%)