Phosphorodifluoridous acid, ethylene ester (8CI) synthesis

Yield: 90%

Reaction Conditions:

with methylmagnesium chloride;antimony(III) fluoride in 2-methyltetrahydrofuran at 60 - 90;Inert atmosphere;Large scale;Solvent;Reagent/catalyst;Temperature;

Steps:

2.1; 3.2 Second step: Synthesis of 1,2-bis(difluorophosphino)ethane
A 100 L lining PTFE reactor was charged with antimony trifluoride 12.02 Kg (67.2 mol, 1.6 eq), 3.0 M methylmagnesium chloride.(0.02 eq) and dried 2-methyltetrahydrofuran 70Kg, heated to 90 ° C for 2 hours, then cooled to 60 ° C, dripAddition of 1,2-bis(dichlorophosphinooxy)ethane 11.08 Kg (1 eq) and 2-methyltetrahydrofuran treated with methylmagnesium chloride85Kg, after the end of the addition, the reaction was incubated for 8 to 9 hours, and the GC sampling test ended. Cooling, reaction hydraulic filtration, filter cake3Kg of 2-methyltetrahydrofuran treated with methylmagnesium chloride was rinsed, the filtrate was concentrated, and then decompressed at 50 ° C / 180 mmHgDistillation gave 7.28 Kg of 1,2-bis(difluorophosphino)ethane in a yield of 90%. The GC purity was 99.5%. Chlorine impurity is less than0.02%, cyclized impurities less than 0.06%. Store under refrigeration with nitrogen.

References:

Pulasi Science And Technology (Shanghai) Co., Ltd.;Lu Dianyun;Cai Weibing;Qi Weijun CN109369707, 2019, A Location in patent:Paragraph 0038-0045; 0046; 0049-0050