反应详情

温度

160 °C

To a flask containing 7-hydroxy-4-methoxy-6-azaindole (0.200 g, 1.22 mmol) was added anisole (3 mL) and then POBr3 (1.57 g, 6.09 mmol). The system was purged with Ar and then it was heated at 160° C. (oil bath temperature) for 1 h. The reaction mixture was then allowed to cool to room temperature, quenched with 2M HBr (5 mL) and extracted with methyl t-butyl ether. The aqueous phase was separated and the pH was adjusted to 6-7, after which it was extracted with EtOAc. The resulting organic phase was dried (MgSO4) and evaporated to give a solid residue which was chromatographed (SiO2/5% MeOH-DCM) to afford the title compound (0.076 g, 27%) as a white solid:

1. customThe system was purged with Ar
2. temperatureto cool to room temperature
3. customquenched with 2M HBr (5 mL)
4. extractionextracted with methyl t-butyl ether
5. customThe aqueous phase was separated
6. extractionafter which it was extracted with EtOAc
7. dry with materialThe resulting organic phase was dried (MgSO4)
8. customevaporated
9. customto give a solid residue which
10. customwas chromatographed (SiO2/5% MeOH-DCM)