反应详情

温度

-70 °C

To a solution of 6-bromo-2,2-dimethyl-2H-benzo[b]pyran (see J. Med. Chem., 33, 3028 [1990]) (5.0 g) in dry tetrahydrofuran (100 ml) at -70° C. under nitrogen was added, dropwise, a 1.6M solution of n-butyllithium in hexane (17 ml). The reaction mixture was stirred at -70° C. for 15 minutes then treated with an excess of finely ground solid CO2. The reaction was further stirred for one hour, the solvent evaporated in vacuo and the residue taken up in ethyl acetate and washed with dilute aqueous hydrochloric acid. The organic layer was concentrated in vacuo to a solid which was triturated with hexane to provide a white solid, 1.6 g.

1. stirringThe reaction was further stirred for one hour
2. customthe solvent evaporated in vacuo
3. washwashed with dilute aqueous hydrochloric acid
4. concentrationThe organic layer was concentrated in vacuo to a solid which
5. customwas triturated with hexane
6. customto provide a white solid, 1.6 g