반응 #77973

반응 방정식

p-dichlorobenzene

AlCl3

acetyl chloride

→

2,5-dichloroacetophenone

용매

water

반응 조건

후처리

1. 1
   온도reflux condenser
2. 2
   기타a clear solution slowly resulting
3. 3
   온도After cooling to room temperature
4. 4
   기타The temperature of the mixture is kept between 30 and 40° C. during the hydrolysis by external cooling
5. 5
   기타After separation of the phases
6. 6
   세척the lower, organic phase is washed with 400 ml of water
7. 7
   기타after fresh phase separation
8. 8
   workup.DISTILLATIONsubjected to fractional distillation

실험 절차

147 g (1.0 mol) of p-dichlorobenzene are completely melted at 60° C. in an apparatus having an attached dropping funnel, stirrer and reflux condenser. 120 g (0.9 mol) of anhydrous AlCl3 are added to the melt. 39.3 g (0.5 mol) of acetyl chloride are then added dropwise to the readily stirrable suspension at 60° C. in the course of about 1 hour, a clear solution slowly resulting. After heating to 110° C., the mixture is stirred at this temperature for 7 hours. After cooling to room temperature, the brown reaction mass is hydrolysed by cautious decantation onto a mixture of 200 ml of water and 200 g of ice. The temperature of the mixture is kept between 30 and 40° C. during the hydrolysis by external cooling. After separation of the phases, the lower, organic phase is washed with 400 ml of water and, after fresh phase separation, subjected to fractional distillation. The aqueous phases are discarded.

출처