反应详情

温度

-40 °C

To a solution of 4.03 g (0.025 mol) of 2-nitro-1-phenyl-1-propene dissolved in 30 ml of dry THF (cooled to -40° C. with an acetronitrile-dry ice bath) and under a positive nitrogen atmosphere was added with stirring 22 ml (0.05 mol) of a 5% ether solution of methyllithium. The resulting solution was stirred for 1 h at -40° C. followed by the addition of 4.9 g (0.025 mol) of tetranitromethane. The solution was then allowed to warm to room temperature and stirred an additional hour. The resulting product was isolated and purified as described in Example 1 above, yielding 3.4 g (60% yield) of an analytically pure white crystalline product, mp 76°-78° C. A similar procedure was used for the preparation of derivatives wherein R3 (see structure above or scheme) was CH3 (CH2)3 and R2 was H and wherein R3 was CH3 and R2 was CH3 (see scheme).

1. additionwas added
2. temperatureto warm to room temperature
3. stirringstirred an additional hour
4. customThe resulting product was isolated
5. custompurified
6. customyielding 3.4 g (60% yield) of an analytically pure white crystalline product, mp 76°-78° C
7. customA similar procedure was used for the preparation of derivatives wherein R3 (see structure above or scheme)