反应详情

温度

115 °C

A mixture of 4-bromo-7-chloro-6-azaindole (1 g), CuI (0.65 g) and NaOMe (4 mL, 25% in methanol) in MeOH (16 mL) was heated at 110-120° C. for 16 hours in a sealed tube. After cooling to room temperature, the reaction mixture was neutralized with 1N HCl to pH 7. The aqueous solution was extracted with EtOAc (3×30 mL). Then the combined organic layer was dried over MgSO4, filtered and the filtrate was concentrated in vacuo to afford a residue, which was purified by using silica gel chromatography to give 0.3 g of 4-methoxy-7-chloro-6-azaindole, Precursor 2e. MS m/z: (M+H)+ calcd for C8H8ClN2O: 183.03; found 183.09. HPLC retention time: 1.02 minutes (column B).

1. temperatureAfter cooling to room temperature
2. extractionThe aqueous solution was extracted with EtOAc (3×30 mL)
3. dry with materialThen the combined organic layer was dried over MgSO4
4. filtrationfiltered
5. concentrationthe filtrate was concentrated in vacuo
6. customto afford a residue, which
7. customwas purified