51738-07-9

945543-21-5

51738-07-9

b) Synthesis of 2-chloro-6-iodobenzaldehyde: 5.14 mL (72.4 mmol) of dimethylsulfoxide dissolved in 15 mL of methylene chloride was slowly added dropwise over 20 min to 3.11 mL (36.2 mmol) of oxalyl chloride dissolved in 40 mL of methylene chloride at -78 °C. The reaction mixture was continued to be stirred at -78°C for 15 minutes before 8.10 g (3.02 mmol) of a solution of 2-chloro-6-iodobenzyl alcohol dissolved in 40 mL of methylene chloride was added dropwise over 30 minutes. After the dropwise addition was completed, the mixture continued to be stirred at -78°C for 45 minutes. Subsequently, 20.9 mL (151 mmol) of triethylamine was slowly added to gradually warm the reaction mixture to room temperature. Upon completion of the reaction, it was quenched by the addition of water and the organic and aqueous phases were separated. The organic phase was dried with anhydrous sodium sulfate, filtered and concentrated under reduced pressure to afford 8.35 g (100% yield) of a yellow crystalline solid 2-chloro-6-iodobenzaldehyde, which was used directly in the next reaction without further purification. Mass spectrometry (EI) data: 268.0 (44%), 266.0 (100%) (M+?) .