反应详情

60% NaH (13 mg, 0.33 mmol) was added to a stirred solution of 7-hydroxy-2-(4-methyl-pyridin-3-yl)-3,4-dihydro-2H-isoquinolin-1-one (27A: 70 mg, 0.275 mmol) in DMF (2 mL) at 0° C. The reaction mixture was stirred at room temperature for 1 hour. This was followed by the addition of 2-chloro-5-fluoro-pyrimidine (44 mg, 0.33 mmol) at 0° C. and stirring was continued for a further 1 hour at room temperature. The reaction was monitored by TLC (5% methanol in DCM). The reaction mixture was quenched with chilled water and extracted with ethylacetate. The organic layer was washed with brine solution, dried over Na2SO4 and concentrated. Purification by column chromatography on silica gel (2% methanol in DCM) afforded 10 mg of the product (10.4% yield).

1. stirringstirring
2. waitwas continued for a further 1 hour at room temperature
3. customThe reaction mixture was quenched with chilled water
4. extractionextracted with ethylacetate
5. washThe organic layer was washed with brine solution
6. dry with materialdried over Na2SO4
7. concentrationconcentrated
8. customPurification by column chromatography on silica gel (2% methanol in DCM)