反应详情

温度

100 °C

Compound 9 (2.0 g, 6.41 mmol., 1.0 eq.), K2CO3 (1.77 g, 12.82 mmol., 2.0 eq.), halide (5.28 g, 32.05 mmol., 5.0 eq.) and DMF (25.0 mL) were combined and heated to 100° C. overnight. The crude reaction mixture was mixed with H2O (30 mL) and CH2Cl2 (35 mL). The organic phase was separated and the aqueous phase was washed with CH2Cl2 (2×25 mL). The combined organic phase was washed with brine and concentrated. The crude material was purified on a silica column to give compound 10 (1.2 g). The structure was confirmed by 1H NMR and LC/MS.

1. customThe crude reaction mixture
2. customThe organic phase was separated
3. washthe aqueous phase was washed with CH2Cl2 (2×25 mL)
4. washThe combined organic phase was washed with brine
5. concentrationconcentrated
6. customThe crude material was purified on a silica column