反应详情

A mixture of tetrachlorosilane (10.07 mmol, 2 mL), NaN3 (30.21 mmol, 1.96 g) and 5-acetylamino-4′-methyl-biphenyl-3-carboxylic acid methyl ester (3.36 mmol, 950.9 mg) in 10 ml of dry acetonitrile was stirred at room temperature for 16 hours. The reaction mixture were poured into ice-cold aqueous Na2CO3 solution and extracted with ethyl acetate (100 mL). The organic layer was washed with brine, dried over anhydrous Na2SO4, filtered, and concentrated in vacuo. The resulting crude 4′-methyl-5-(5-methyl-tetrazol-1-yl)-biphenyl-3-carboxylic acid methyl ester was used for next step directly (880 mg, 85% yield).

1. additionThe reaction mixture were poured into ice-cold aqueous Na2CO3 solution
2. extractionextracted with ethyl acetate (100 mL)
3. washThe organic layer was washed with brine
4. dry with materialdried over anhydrous Na2SO4
5. filtrationfiltered
6. concentrationconcentrated in vacuo