Calcium phosphorylcholine chloride synthesis

Yield:4826-71-5 100 g

Reaction Conditions:

Stage #1:choline chloride with phosphoric acid at 25 - 120; for 6 h;
Stage #2: with calcium hydroxide in water at 25; for 0.166667 h;

Steps:

1 Preparation Example 1
1) 140 g of phosphoric acid was added slowly (at a dropping rate of 10 drops / s) to 100 g of crude choline chloride (containing 70% choline chloride) at 25 °C and -0.09 MPa, After the addition was completed, the temperature was raised to 70 ° C. and vacuum distillation was carried out until no distilled water was obtained, then the temperature was raised to 120 °C. and the reaction pressure was controlled at -0.09 MPa for 6 h, and then 50 g of water was added to terminate the reaction to obtain a phosphorylcholine chloride mixture. 2) mixing 100 g of the above mixture of phosphoryl choline chloride with 3000 g of calcium hydroxide aqueous solution (mass fraction of calcium hydroxide being 15%) at 25 ° C. for 10 min until the pH of the system reaches 8 to obtain metathesis mixture; 3) subjecting the metathesis mixture to vacuum distillation at 25 ° C. and 35 Pa until solid precipitates to obtain a solid-liquid mixture; 4) The solid-liquid mixture was cooled to -5 crystallization 40min, then filtered and dried at 100 2h obtained 100g chlorophosphorylcholine calcium salt tetrahydrate (purity 100%), 5) The filtrate was filtered at -5 °C. recrystallization 40min, then filtered and dried at 100° C. 2h to obtain chlorophosphorylcholine calcium salt tetrahydrate compounds.

References:

Wuhu Fu Min Biological Pharmaceutical Co., Ltd.;Su Funan CN104926862, 2017, B Location in patent:Paragraph 0056-0061

FullText