反应详情

温度

-78 °C

Dissolve 7-bromo-thieno[3,2-b]pyridine (3.69 g, 17 mmol) in dry THF (20 mL) and cool to −78° C. Add n-BuLi (1.6 M in hexane, 21.2 mL, 34 mmol) slowly to the mixture at −78° C. and stir at −78° C. for 20 min. Add MeOH/H2O=1/1 (20 mL) and stir at room temperature for 1 h. Extract the reaction mixture with CH2Cl2. Wash the organic portion with saturated NaCl solution, dry over Na2SO4, and evaporate. Purify the resulting residue using silica gel chromatography, eluting with 100% hexane to hexane:ethyl acetate=10:1 to give the title compound (1.44 g, 62%). ES/MS m/z 136 (M+1)+.

1. extractionExtract the reaction mixture with CH2Cl2
2. washWash the organic portion with saturated NaCl solution
3. dry with materialdry over Na2SO4
4. customevaporate
5. customPurify the resulting residue
6. washeluting with 100% hexane to hexane