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ChemicalBook CAS DataBase List DIETHYL 1-TETRADECANEPHOSPHONATE
5191-09-3

DIETHYL 1-TETRADECANEPHOSPHONATE synthesis

3synthesis methods
-

Yield:5191-09-3 95.1%

Reaction Conditions:

with di-tert-butyl peroxide;silver(I) fluoride at 149; for 5 h;Inert atmosphere;

Steps:

4 Example 4

A mixture of 1077 g of diethyl phosphite and 0.69 g of silver fluoride was heated to 149°C with stirring in a 3000 mL reaction flask equipped with a stirrer, thermometer, peristaltic pump feeder, nitrogen gas duct and condenser. After reaching this temperature, open the peristaltic pump, slowly add 70g initiator di-tert-butyl peroxide and 1180g 1-tetradecene to above-mentioned system, the initiator feeding speed must be controlled to ensure that the reaction system temperature is maintained at 149 ± 1 is appropriate. After the feed of initiator di-tert-butyl peroxide and 1-tetradecene was completed, the reaction was continued at 149° C. for 5 hours. The reaction progress is monitored by gas chromatography analysis, and the end point of the reaction is determined by the disappearance of the chromatographic peak of the raw material 1-tetradecene, and the complete conversion to the chromatographic peak of the target product 1-tetradecylphosphonate diethyl ester. The excess diethyl phosphite was removed by distillation under reduced pressure and filtered to obtain the target product, diethyl 1-tetradecylphosphonate (purity 99.2% (GC), yield 95.1%).

References:

CN114149463,2022,A Location in patent:Paragraph 0052-0053

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