2-甲基-2,5-二氮杂双环(2.2.2)辛烷

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: A solution of 2-benzoyl-5-methyl-2,5-diazabicyclo[2.2.2]octane (17.2 g, 0.074 mole) in concentrated hydrochloric acid (172 ml) was refluxed 48 hours. The solution was evaporated to dryness in vacuo and the residue triturated with diethyl ether. The supernatant, after centrifugation, was decanted, and the procedure was repeated using absolute ethanol. The hygroscopic residue of 2-methyl-2,5-diazabicyclo[2.2.2]octane . 2HCl (12.1 g, 81.5%) was dried in vacuo. It slowly decomposed above 300°C. The solution was evaporated to dryness in vacuo the residue triturated with diethyl ether The supernatant, after centrifugation, was decanted The hygroscopic residue of 2-methyl-2,5-diazabicyclo[2.2.2]octane . 2HCl (12.1 g, 81.5%) was dried in vacuo It slowly decomposed above 300°C.

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: A solution of 2-benzoyl-5-methyl-2,5-diazabicyclo[2.2.2]octane (17.2 g, 0.074 mole) in concentrated hydrochloric acid (172 ml) was refluxed 48 hours. The solution was evaporated to dryness in vacuo and the residue triturated with diethyl ether. The supernatant, after centrifugation, was decanted, and the procedure was repeated using absolute ethanol. The hygroscopic residue of 2-methyl-2,5-diazabicyclo[2.2.2]octane . 2HCl (12.1 g, 81.5%) was dried in vacuo. It slowly decomposed above 300°C. The solution was evaporated to dryness in vacuo the residue triturated with diethyl ether The supernatant, after centrifugation, was decanted The hygroscopic residue of 2-methyl-2,5-diazabicyclo[2.2.2]octane . 2HCl (12.1 g, 81.5%) was dried in vacuo It slowly decomposed above 300°C.

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: A solution of 2-benzoyl-5-methyl-2,5-diazabicyclo[2.2.2]octane (17.2 g, 0.074 mole) in concentrated hydrochloric acid (172 ml) was refluxed 48 hours. The solution was evaporated to dryness in vacuo and the residue triturated with diethyl ether. The supernatant, after centrifugation, was decanted, and the procedure was repeated using absolute ethanol. The hygroscopic residue of 2-methyl-2,5-diazabicyclo[2.2.2]octane . 2HCl (12.1 g, 81.5%) was dried in vacuo. It slowly decomposed above 300°C. The solution was evaporated to dryness in vacuo the residue triturated with diethyl ether The supernatant, after centrifugation, was decanted The hygroscopic residue of 2-methyl-2,5-diazabicyclo[2.2.2]octane . 2HCl (12.1 g, 81.5%) was dried in vacuo It slowly decomposed above 300°C.

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: A solution of 2-benzoyl-5-methyl-2,5-diazabicyclo[2.2.2]octane (17.2 g, 0.074 mole) in concentrated hydrochloric acid (172 ml) was refluxed 48 hours. The solution was evaporated to dryness in vacuo and the residue triturated with diethyl ether. The supernatant, after centrifugation, was decanted, and the procedure was repeated using absolute ethanol. The hygroscopic residue of 2-methyl-2,5-diazabicyclo[2.2.2]octane. 2HCl (12.1 g, 81.5%) was dried in vacuo. It slowly decomposed above 300° C. The solution was evaporated to dryness in vacuo the residue triturated with diethyl ether The supernatant, after centrifugation, was decanted The hygroscopic residue of 2-methyl-2,5-diazabicyclo[2.2.2]octane. 2HCl (12.1 g, 81.5%) was dried in vacuo It slowly decomposed above 300° C.

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: A solution of 2-benzoyl-5-methyl-2,5-diazabicyclo[2.2.2]octane (17.2 g, 0.074 mole) in concentrated hydrochloric acid (172 ml) was refluxed 48 hours. The solution was evaporated to dryness in vacuo and the residue triturated with diethyl ether. The supernatant, after centrifugation, was decanted, and the procedure was repeated using absolute ethanol. The hygroscopic residue of 2-methyl-2,5-diazabicyclo[2.2.2]octane . 2HCl (12.1 g, 81.5%) was dried in vacuo. It slowly decomposed above 300°C. The solution was evaporated to dryness in vacuo the residue triturated with diethyl ether The supernatant, after centrifugation, was decanted The hygroscopic residue of 2-methyl-2,5-diazabicyclo[2.2.2]octane . 2HCl (12.1 g, 81.5%) was dried in vacuo It slowly decomposed above 300°C.