反应详情

A mixture of 2',3',4'-trichloroacetophenone (21.4 g, 0.0958 mole), anhydrous sodium acetate (8.0 g), and n-hexane (50 ml) was heated under reflux while treated with a solution of bromine (15.3 g, 0.096 mole) in 25 ml of n-hexane in five portions, decolorizing before each new addition. The mixture was then filtered while hot and the insoluble residue was triturated twice with 50 ml of boiling n-hexane. Enough additional n-hexane was added to the combined filtrates to avoid oiling out of product at 40°. The solution was then seeded and cooled at -10° for 18 hours. Product was collected and air dried to give 17.9 g (62%), mp 44°-46°.

1. temperaturewas heated
2. temperatureunder reflux
3. additiondecolorizing before each new addition
4. filtrationThe mixture was then filtered while hot and the insoluble residue
5. customwas triturated twice with 50 ml of boiling n-hexane
6. additionEnough additional n-hexane was added to the combined filtrates
7. customto avoid oiling out of product at 40°
8. temperaturecooled at -10° for 18 hours
9. customProduct was collected
10. customair dried
11. customto give 17.9 g (62%), mp 44°-46°