[3-(Dimethylamino)propyl]triphenylphosphonium bromide hydrobromide synthesis

Yield:27710-82-3 92.4%

Reaction Conditions:

in ethanol;Reflux;Temperature;

Steps:

17-32; 2 Comparative Example 2. Synthesis of [3-(Dimethylamine)propyl]triphenylphosphonium bromide hydrobromide

General procedure: Add 720 g of absolute ethanol to the reaction flask, add about 300 g of 123B1-10 obtained in Comparative Example 1, add 450 g of 40% dimethylamine aqueous solution, and heat and reflux for 4 to 5 hours; after the reaction is completed, concentrate the dry solvent under reduced pressure to obtain Add 400g of anhydrous ethanol to the residue, stir and heat to reflux to disperse the agglomerated solids; cool and crystallize; filter, collect the solids and dry to obtain about 273g of the product 123B2-10. Single-pass yield: 82.9%. HPLC: 99.92%; where: 123B2-10: triphenylphosphine: 123B1-X2=99.97:0.00:0.03 (excluding other impurities).The mother liquor is collected and recovered to obtain about 31 g of the product 123B2-10. Recovery rate: 9.4%. HPLC: 99.63%; where: 123B2-10: triphenylphosphine: 123B1-X2=99.92:0.00:0.08 (excluding other impurities).A total of about 304g of 123B2-10 is obtained. The total yield of ammonolysis: 92.4%.

References:

CN111548369,2020,A Location in patent:Paragraph 0048-0072; 0076-0083