2-methyl-2-propylpropane-1,3-diyl dinitrate synthesis

Yield:10605-24-0 90%

Reaction Conditions:

with nitric acid;acetic anhydride at 15 - 20; for 1 h;

Steps:

Synthesis of 2-methyl-2-[(nitrooxy)methyl]pentyl nitrate and 2-propylpentyl nitrateThe following provides a synthesis for 2-methyl-2-[(nitrooxy)methyl]pentyl nitrate. 22 mmole of concentrated nitric acid dropwise into 10 mL of acetic anhydride under stirring and cooling in an ice bath. Following the addition of the nitric acid, 20 mmole of an alkyl alcohol was added in small amounts to the solution with cooling at 15° C. and allowed to react at room temperature for an hour. The reaction mixture was poured into 100 mL of ice cold water. The product was then extracted with 2×25 ml ether. The organic layer was collected and washed with 2×10 ml saturated sodium bicarbonate solution and then 3×10 mL water. The organic layer was dried over MgSO4 and concentrated by evaporation. The yield was over 90%. An NMR spectra of 2-methyl-2-[(nitrooxy)methyl]pentyl nitrate and 2-propylpentyl nitrate is shown in FIGS. 1 and 2.

References:

US2011/130455,2011,A1 Location in patent:Page/Page column 5