反应详情

Add a solution of 3-(4-benzyl-2-methylpiperazin-1-yl)-6-(4-fluorophenyl)-4,5-dimethylpyridazine (200 mg, 3.25 mmol) in absolute EtOH (15 mL) to 10% Pd/C (46.8 mg) pre-wetted with EtOH (5 mL). Shake the mixture in a Parr bottle pressurized with H2 at 60 psi for 10 h. Filter the reaction mixture, and apply the solution directly to an SCX column (Varian, 2 g). Rinse the column with MeOH and CH2Cl2. Elute the product with a 1:1 mixture of 2 M NH3/MeOH and CH2Cl2. Concentrate the eluent under reduced pressure to afford the title compound as an off-white foam (142 mg, 92%). ES/MS m/z 301.2 (M+1).

1. filtrationFilter the reaction mixture
2. washRinse the column with MeOH and CH2Cl2
3. washElute the product
4. additionwith a 1:1 mixture of 2 M NH3/MeOH and CH2Cl2
5. concentrationConcentrate the eluent under reduced pressure