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.
The TCP and TEA dissolved in the toluene
Solution was cooled down in an ice bath
Addition of the oxalyl chloride
The precipitated product
The crude TCPO