反应详情

To a cooled (0° C.) solution of 11a (500 mg, 2.7 mmol) in DMF (30 ml), NaH (130 mg, 3.2 mmol) was added. The mixture was stirred for 10 min. and a solution of p-toluensulphonyl chloride (570 mg, 3.0 mmol) in DMF (10 ml) was added. The mixture was stirred at room temperature for 1 h. and quenched with water (1 ml). The solvent was evaporated and the residue dissolved in AcOEt. The organic solution was washed with aq. Na2CO3, evaporated and purified by flash column chromatography. Elution with hexane/CH2Cl2 (1/1) gave 8,9-dihydro-8-(4methylphenylsulfonyl)pyrido[3′,2′:4,5]-pyrrolo[1,2-c]pyrimidin-9-one (360 mg, 40%) as a white solid.

1. additionwas added
2. stirringThe mixture was stirred at room temperature for 1 h.
3. customquenched with water (1 ml)
4. customThe solvent was evaporated
5. dissolutionthe residue dissolved in AcOEt
6. washThe organic solution was washed with aq. Na2CO3
7. customevaporated
8. custompurified by flash column chromatography
9. washElution with hexane/CH2Cl2 (1/1)