Synthesis of Bis(2,4,6-trichlorophenyl) oxalate (TCPO)

7 g of dried 2,4,6-trichlorophenol is dissolved in 60 mL of anhydrous toluene, add 5.6 mL of triethylamine then cool the solution down in an ice bath. A slow addition of2 mL of oxalyl chloride is started via a syringe, with vigorous stirring over 10 minutes period of time. The temperature of the solution needs to be kept below 10°C. The mixture is then refluxed for 30 min. Cool the solution down in a freezer, filter and wash with 10 mL of hexane and10 mL of water. Recrystallize in ethyl acetate.

Source

The TCP and TEA dissolved in the toluene

Solution was cooled down in an ice bath

Addition of the oxalyl chloride

The reflux

The precipitated product

The crude TCPO

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