ChemicalBook CAS DataBase List Lithium difluoro(oxalato)borate(1-)

Lithium difluoro(oxalato)borate(1-) synthesis

5synthesis methods

Product Name:Lithium difluoro(oxalato)borate(1-)
CAS Number:409071-16-5
Molecular formula:C2BF2O4.Li
Molecular Weight:143.76

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7664-39-3 Synthesis

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Yield:409071-16-5 99.1%

Reaction Conditions:

Stage #1: oxalyl dichloride;fluoroboronic acid in acetonitrile at -30; under 0 Torr; for 24 h;Flow reactor;
Stage #2: hydrogen fluoride in acetonitrile;Flow reactor;

Steps:

9 Example 9: Preparation and purification method of compound I

To a 1 L dry reactor was added Ligand Compound a, Compound II and the reaction solvent acetonitrile under stirring.The molar ratio of the ligand compound a to the compound II is 1:1, the reaction temperature is -30 ° C, the reaction pressure is 0 MPa (gauge pressure), the reaction time is 24 hours, and the crude product A is obtained, and the crude product A is further subjected to HF fluorination. reaction.After the completion of the reaction, the mixture was cooled to room temperature, and the insoluble material was filtered. The solvent was evaporated to remove the solvent, and the crystals were concentrated and dried to give a crude compound I. The crude product of the compound I was 99.6% and the crude product was 92%.The recrystallization solvent was acetonitrile, and the other reaction conditions were the same as in Example 1.The purity of the boutique is 99.99% and the total yield is 99.1%. The product has a chloride ion content <10ppm, a fluoride ion content <10ppm, a sulfate content <10ppm, a moisture content <10ppm, a metal content <10ppm, and other impurities <10ppm.

References:

CN109467539,2019,A Location in patent:Paragraph 0206-0209

553-91-3 Synthesis