反应详情

温度

60 °C

Anhydrous aluminum chloride was mixed (5 grams, 37.5 millimoles, 2.4 equivalents) with 1-bromo-2,5 difluorobenzene in a dry, round-bottom flask blanketed with nitrogen and fitted with a condenser. The mixture was heated to 60° C. and acetyl chloride (1.7 milliliters, 23.3 millimole, 1.5. equivalents) was added by syringe. The wet yellow solid changed then into a scarlet solution and was heated at 90° C. for 1 hour. The reaction mixture was poured onto 38 grams of ice, HCl was added (3 milliliters, 37% concentration) and the mixture was extracted with ether. The crude material was dried over magnesium sulfate and evaporated down. The crude material was purified by column chromatography or distilled. The product (1.2 grams, 31%) was obtained as a yellow oil.

1. customfitted with a condenser
2. temperatureinto a scarlet solution and was heated at 90° C. for 1 hour
3. additionwas added
4. concentration(3 milliliters, 37% concentration)
5. extractionthe mixture was extracted with ether
6. dry with materialThe crude material was dried over magnesium sulfate
7. customevaporated down
8. customThe crude material was purified by column chromatography
9. distillationdistilled