反应详情

35 mL of ammonia were condensed into a Schlenk flask, cooled in a dryice-isopropanol bath. 170 mg of sodium were dissolved and 1.1 g of 40, dissolved in 3 mL of dry tetrahydrofurane, were added. After complete conversion, the reaction was quenched by addition of methanol and the mixture was warmed to room temperature. The solvents were evaporated and the crude material was taken up in methanol and dilute hydrochloric acid and evaporated several times to give 1.19 g of crude product as a cis/trans mixture, which was used directly in the next step, Rt=0.10 min (Method P). Detected mass: 188.1 (M+H+).

1. customcondensed into a Schlenk flask
2. temperaturecooled in a dryice-isopropanol bath
3. additionwere added
4. customAfter complete conversion, the reaction was quenched by addition of methanol
5. customThe solvents were evaporated
6. customdilute hydrochloric acid and evaporated several times