反应详情

To a stirred solution of 15 g (0.1 mole) of 2,2-dinitropropanol and 1.5 g (0.05 mole) of s-trioxane in 13 mL of methylene chloride at 0° C., 15 g (98%) of a concentrated sulfuric acid solution was injected with syringe pump over 2 hours. During the reaction, temperature was controlled not to exceed 5° C. After addition was completed, the reaction was stirred for further 30 minutes. Upon completion of the reaction, the reaction solution was quenched with water. The reaction mixture was extracted with 130 mL of methylene chloride, and then, the extract was successively washed with 5% sodium hydroxide aqueous solution (130 mL×4) and saturated sodium chloride aqueous solution (130 mL×2), dried over anhydrous magnesium sulfate, and then filtered. The filtrate was concentrated under reduced pressure. Further evaporation under 60° C., about 10 mmHg for 5 hours gave 12.8 g of BDNPF.

1. customDuring the reaction, temperature
2. customto exceed 5° C
3. additionAfter addition
4. customUpon completion of the reaction
5. customthe reaction solution was quenched with water
6. extractionThe reaction mixture was extracted with 130 mL of methylene chloride
7. washthe extract was successively washed with 5% sodium hydroxide aqueous solution (130 mL×4) and saturated sodium chloride aqueous solution (130 mL×2)
8. dry with materialdried over anhydrous magnesium sulfate
9. filtrationfiltered
10. concentrationThe filtrate was concentrated under reduced pressure
11. customFurther evaporation under 60° C.