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HRID 1357441作成日:2026年10月26日

Sulfuric Acid → Propane, 1,1'-[methylenebis(oxy)]bis[2,2-dinitro-

https://huagongshe.com/reaction/1357441

反応式

関与物質

役割名称HCID仕込み量
反応物Sulfuric AcidHCID 1118—
反応物1,3,5-TrioxaneHCID 8081—
反応物2,2-DinitropropanolHCID 70194—
溶媒DichloromethaneHCID 6344—
生成物Propane, 1,1'-[methylenebis(oxy)]bis[2,2-dinitro-HCID 8001587%

反応手順

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.

情報源と証拠

DOI10.6084/m9.figshare.5104873.v1
特許番号US06592692B2
出典データセットuspto-grants-2003_07
ORD IDord-8cf56cb6243241e9b1ce4dd0f0f0e196
出典メモuspto-grants-2003_07