Yield:631-45-8 88%

Reaction Conditions:

Stage #1: ortho-cresolwith potassium phosphate;diphenyl diselenide;phosphorus in dimethyl sulfoxide;toluene at 60; for 4 h;Inert atmosphere;
Stage #2: with sulfur in dimethyl sulfoxide;toluene at 60; for 4 h;Inert atmosphere;

Steps:

30 Example 30: Preparation of tri-o-methylphenyl thiophosphate

In a 10mL reaction flask, first add K3PO4 (0.045mmol, 9.6mg), diphenyl diselenide (0.045mmol, 14.1mg), White phosphorus toluene solution (white phosphorus 5.6mg, toluene 0.5mL), o-methylphenol (1.1mmol, 117.0mg), dimethyl sulfoxide (0.5mL), under argon conditions, The temperature was raised to 60 °C, and after 4 hours of reaction, sulfur powder (11mg) was added at 60 °C, and after 4 hours of reaction, the reaction was completed by phosphorus spectrum detection, and the reaction was stopped.The reaction solution was concentrated and separated by column chromatography to obtain 60.9 mg of tri-o-methyl phenyl thiophosphate, with a yield of 88%

References:

CN113004323,2021,A Location in patent:Paragraph 0065-0067