反应详情

The crude product of example 2 was dissolved in DMF (50 ml) and then K2CO3 (3.3 g, 0.024 mol) was added. After stirring at room temperature for about 0.5 hours, benzyl bromide (4.0 g, 0.0234 mol) was added drop-wise. Then the mixture was heated at 80° C. for another 5 hours. After cooling to room temperature, the solids were filtered off and washed with ethyl acetate. The filtrate was diluted with EA, washed with water and then brine, dried and concentrated. The residue was purified by column chromatography (CH2Cl2/MeOH=50/1) to give the titled compound (2.0 g, 2-step yield 49.3%).

1. temperatureThen the mixture was heated at 80° C. for another 5 hours
2. temperatureAfter cooling to room temperature
3. filtrationthe solids were filtered off
4. washwashed with ethyl acetate
5. additionThe filtrate was diluted with EA
6. washwashed with water
7. dry with materialbrine, dried
8. concentrationconcentrated
9. customThe residue was purified by column chromatography (CH2Cl2/MeOH=50/1)