反应详情

温度

60 °C

Into a 250 ml round bottom flask equipped with a stir bar, thermometer and reflux condenser topped with a nitrogen inlet was added 5.73 (0.03) mole) of 2,2-dimethyl-5-hydroxymethyl-5-nitro-1,3-dioxane and 70 ml 10% sodium hydroxide which was heated to 60° C. for one hour. The solution was cooled to 5° C. and at this temperature acidified to pH 5 with concentrated acetic acid. The precipitated solid was filtered off and dried to give 5.2 g (92%) of 2,2-dimethyl-5-nitro-1,3-dioxane m.p. 60°-61° C. 1H NMR in CD3OD also confirmed the structure.

1. customInto a 250 ml round bottom flask equipped with a stir bar
2. temperaturethermometer and reflux condenser
3. customtopped with a nitrogen inlet
4. temperatureThe solution was cooled to 5° C. and at this temperature
5. filtrationThe precipitated solid was filtered off
6. customdried