反应详情

A mixture of 2-(6-methylpyridazin-3-yl)-2,4,6,7-tetrahydro-5H-pyrazolo[4,3-c]pyridine hydrochloride (920 mg, 3.65 mmol), 1-(chloroacetyl)-4-cyclobutylpiperazine (791 mg, 3.65 mmol), K2CO3 (2.52 g, 18.3 mmol) and KI (66 mg, 0.4 mmol) in CH3CN (20 ml) is stirred at rt overnight. The solvent is removed in vacuo and the residue is partitioned between water (20 mL) and EtOAc (20 mL). The layers are separated and the aqueous layer is extracted with EtOAc (3×20 mL). The combined extracts are washed with brine (30 mL), dried and evaporated. The resulting oil is purified by flash column with DCM/MeOH/NH4OH (100:5:0.5) to give the title compound as a light yellow solid. 1H NMR (δ, CDCl3): 8.43 (s, 1H), 8.01 (d, 1H), 7.41 (d. 1H), 3.64-3.67 (m, 6H), 3.40 (s, 2H), 2.88 (s, 4H), 2.66-2.72 (m, 4H), 2.29 (q, 4H), 1.59-2.05 (m, 6H). MS (M+1): 396.2.

1. customThe solvent is removed in vacuo
2. customthe residue is partitioned between water (20 mL) and EtOAc (20 mL)
3. customThe layers are separated
4. extractionthe aqueous layer is extracted with EtOAc (3×20 mL)
5. washThe combined extracts are washed with brine (30 mL)
6. customdried
7. customevaporated
8. customThe resulting oil is purified by flash column with DCM/MeOH/NH4OH (100:5:0.5)