反应详情

6-Bromo-4-(bromomethyl)-2-(phenylsulfonyl)isoquinolin-1(2H)-one (Example 11d, 2.0 g), tert-butyl (3R)-3-methylpiperazine-1-carboxylate (0.946 g) and N,N-diisopropylethylamine (1.143 mL) were dissolved in THF (10 mL) and stirred at room temperature under nitrogen for 16 h. The reaction mixture was diluted with methanol (10 mL) and treated with sodium hydroxide (0.35 g), after stirring at room temperature for 1 h, water (200 mL) was added and the reaction mixture extracted into ethyl acetate (250 mL). The separated organic layer was dried (MgSO4) filtered and evaporated, the residue was purified (SiO2 chromatography, elution with ethyl acetate) to give the subtitle compound (0.75 g) as a solid.

1. stirringafter stirring at room temperature for 1 h
2. extractionthe reaction mixture extracted into ethyl acetate (250 mL)
3. dry with materialThe separated organic layer was dried (MgSO4)
4. filtrationfiltered
5. customevaporated
6. customthe residue was purified
7. wash(SiO2 chromatography, elution with ethyl acetate)