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Diphenylfluorophosphine oxide synthesis

12synthesis methods
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Yield:1135-98-4 97%

Reaction Conditions:

with potassium 2-(difluoro(trifluoromethoxy)methoxy)-2,2-difluoroacetate in N,N-dimethyl-formamide at 80; for 1 h;Schlenk technique;Inert atmosphere;Reagent/catalyst;Temperature;Solvent;

Steps:

77-104; 112-148

Weigh the phosphoric acid substrate 4-3a (0.2mmol, 1.0equiv) and the fluorinating reagent CF3OCF2OCF2CD2K (OC2K) (0.11mmol, 0.55equiv) in a 10mL dried Shrek tube, pump out the nitrogen three times, and add it under the protection of nitrogen Anhydrous DMF 1mL, react at 80°C for 1h. After the reaction, the reaction product was cooled to room temperature and filtered to obtain the reaction product. The reaction product was added with 15 mL of water, and 15 mL of ethyl acetate (or dichloromethane) was added for extraction three times. The layers were separated, the organic phase was collected, and the organic phases were combined. Na2S04 was dried, concentrated, and purified by silica gel column chromatography to obtain the final product.

References:

CN112174761,2021,A Location in patent:Paragraph 0169-0212; 0215-0268