2-ethyl-2-nitropropane-1,3-diol

反応条件: temp:0.00; pressure:0.00; stir:

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: 7.46 g of 2-nitro-2-ethyl-1,3-propanediol, 8.61 g of butyl levulinate, 50 mg of p-toluenesulfonic acid in 50 ml of toluene was refluxed until no more water separated. The reaction mixture was cooled, washed with 2% sodium bicarbonate and water, dried and concentrated to give 13.65 g of 2-carbobutoxyethyl-2-methyl-5-nitro-5-ethyl-1,3-dioxane as a light yellow oil. This was dissolved in 50 ml of ethanol and hydrogenated over 1 g Raney Nickel catalyst at 60 under pressure. Distillation of the crude material at 160° C./3mm gave 11 g of the product. separated The reaction mixture was cooled washed with 2% sodium bicarbonate and water dried concentrated

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: 7.46 g of 2-nitro-2-ethyl-1,3-propanediol, 8.61 g of butyl levulinate, 50 mg of p-toluenesulfonic acid in 50 ml of toluene was refluxed until no more water separated. The reaction mixture was cooled, washed with 2% sodium bicarbonate and water, dried and concentrated to give 13.65 g of 2-carbobutoxyethyl-2-methyl-5-nitro-5-ethyl-1,3-dioxane as a light yellow oil. This was dissolved in 50 ml of ethanol and hydrogenated over 1 g Raney Nickel catalyst at 60 under pressure. Distillation of the crude material at 160° C./3mm gave 11 g of the product. separated The reaction mixture was cooled washed with 2% sodium bicarbonate and water dried concentrated

反応条件: temp:0.00; pressure:0.00; stir:

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: To a 1 neck round bottom flask equipped with stir bar and dropping funnel capped with a nitrogen outlet was added hexamethylenediamine (HMDA) (20 g, 0.17 mol). A 55% aqueous solution of the mixture of 2-nitro-2-ethyl-1,3-propanediol and 2-ethyl-2-nitrobutanol (189 g, 0.69 mol) was added drop wise to the flask over a period of 1 h with continuous stirring. After complete addition, the dropping funnel was replaced by a condenser and the reaction mixture refluxed for 6 h and stirred at room temperature overnight. After completion of the reaction, the content of the flask was filtered through suction filtration and the deep red high viscous material was collected and dried under vacuum for 8 h. The molecule was too bulky to be detected in GC/MS. The sample was passed through the HPLC Column (90/10 water/acetonitrile) and it showed the formation of three different products. The HPLC retention times recorded were 1.27, 1.66 and 1.91 minutes, with the most polar compound i.e., retention time 1.27 min was formed in greatest amount. To a 1 neck round bottom flask equipped capped with a nitrogen outlet was added drop wise to the flask over a period of 1 h with continuous stirring After complete addition the dropping funnel was replaced by a condenser the reaction mixture refluxed for 6 h stirred at room temperature overnight After completion of the reaction the content of the flask was filtered through suction filtration the deep red high viscous material was collected dried under vacuum for 8 h 1.27, 1.66 and 1.91 minutes with the most polar compound i.e., retention time 1.27 min was formed in greatest amount

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: 7.46 g of 2-nitro-2-ethyl-1,3-propanediol, 8.61 g of butyl levulinate, 50 mg of p-toluenesulfonic acid in 50 ml of toluene was refluxed until no more water separated. The reaction mixture was cooled, washed with 2% sodium bicarbonate and water, dried and concentrated to give 13.65 g of 2-carbobutoxyethyl-2-methyl-5-nitro-5-ethyl-1,3-dioxane as a light yellow oil. This was dissolved in 50 ml of ethanol and hydrogenated over 1 g Raney Nickel catalyst at 60 under pressure. Distillation of the crude material at 160° C./3mm gave 11 g of the product. separated The reaction mixture was cooled washed with 2% sodium bicarbonate and water dried concentrated