反应详情

To a suspension of N-[3-(4-methoxyphenyl)-[1,2,4]triazolo[3,4-a]phthalazin-6-yl]-benzene-1,3-diamine (compound A2) (1.90 g) and DMAP (304 mg) in a 3:1:1 mixture of anhydrous pyridine, anhydrous acetonitrile and anhydrous dichloromethane (100 mL) is added dimethylsulfamoyl chloride (2.67 mL). The mixture is stirred at RT for 3 days and filtered. The filtrate is concentrated in vacuum and a non-saturated solution of NaHCO3 (250 mL) is added to the residue. The suspension is filtered and the solid washed with a minimum of MeOH and AcOEt. Purification of residue by column chromatography (CH2Cl2/MeOH, 98:2) gives 1.43 g of the title compound as white powder.

1. filtrationfiltered
2. concentrationThe filtrate is concentrated in vacuum
3. additiona non-saturated solution of NaHCO3 (250 mL) is added to the residue
4. filtrationThe suspension is filtered
5. washthe solid washed with a minimum of MeOH and AcOEt
6. customPurification of residue by column chromatography (CH2Cl2/MeOH, 98:2)