反应详情

Quinuclidin-3-one (125 g., 1 mole) was dried by azeotropic distillation (40% w/w in toluene) and placed in a 3 l. flask equipped with a mechanical stirrer, 1 l. methanolic sodium ethoxide was added and the clear solution was stirred at 15°-20° C. Nitromethane, 61 g. (1.0 mole), dissolved in 500 ml. absolute ethanol was then added over 0.5 hour while keeping the temperature below 20° C. The solution was acidified to pH=1 using HCl-isopropanol, filtered and dried to yield 160 g. crude product which was used as such for the next step.

1. customflask equipped with a mechanical stirrer
2. dissolution(1.0 mole), dissolved in 500 ml
3. customthe temperature below 20° C
4. filtrationfiltered
5. customdried
6. customto yield 160 g