Iodine → HCID 22641242, compound

Participants

Reaction Conditions

Reaction Steps

Into a 300 ml four-necked flask was placed 31.68 g (0.12 mol) of 1-(3,7-dimethyloctyloxy)-2,5-dimethylbenzene and 10 ml of chloroform and 0.21 g (0.8 mmol) of iodine, and the flask was purged with nitrogen while stirring and the mixture was cooled to 0° C. Bromine in an amount of 19.18 g (0.12 mol) was added dropwise over 1 hour while keeping the temperature not more than 5° C. After addition, the mixture was heated to 30° C. and kept at the same temperature for 5 hours to complete the reaction. The mixture was cooled to room temperature, and the reaction mixture was added into 200 ml of a 5% sodium hydroxide aqueous solution. The mixture was stirred for 10 minutes, then, separated and extracted. The chloroform layer was washed with 200 ml of water, and the organic layer was dried over sodium sulfate. It was concentrated by an evaporator and the resulting residue was purified by column chromatography to obtain 1-(3,7-dimethyloctyloxy)-2,5-dimethyl-4-bromobenzene. The yield amount was 30 g (87.9 mmol) and the yield was 73%.

Provenance & Evidence