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ChemicalBook CAS DataBase List PHENYLPHOSPHONIC ACID DIMETHYL ESTER
2240-41-7

PHENYLPHOSPHONIC ACID DIMETHYL ESTER synthesis

14synthesis methods
-

Yield: 93%

Reaction Conditions:

with caesium carbonate;cesium fluoride in acetonitrile at 100; for 12 h;Sealed tube;

Steps:

4.3. General procedures for the reaction of o-(trimethylsilyl)aryl triflate with dialkyl phosphate
General procedure: In a typical reaction, to an oven-dried 25 mL heavy walled sealtube fitted with Teflon plug valve was added CsF (0.60 mmol),Cs2CO3 (0.90 mmol), o-(trimethylsilyl)aryl triflate (0.30 mmol) anddialkyl phosphate (0.32 mmol). MeCN (3 mL) was added via a syringe. The tube was sealed with Teflon plug valve and then thereaction mixture was stirred at 100 C for 12 h. The reaction wasallowed to cool to room temperature. Then reaction mixture wasdiluted with 5 mL water. The aqueous layer was extracted withethyl acetate (35 mL). The combined organic layers were driedover Na2SO4, filtered and concentrated. The product was isolatedthrough preparative thin-layer chromatography.

References:

Yang, Guoqiang;Shen, Chaoren;Quan, Mao;Zhang, Wanbin [Tetrahedron,2016,vol. 72,# 2,p. 333 - 337] Location in patent:supporting information

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