1,4-Dichlorobenzene → Ethanone, 1-(2,5-dichlorophenyl)-

HRID 49695

반응식

HRID 49695 반응식
[CH:1]1[C:6]([Cl:7])=[CH:5][CH:4]=[C:3]([Cl:8])[CH:2]=1.[Al+3].[Cl-].[Cl-].[Cl-].[C:13](Cl)(=[O:15])[CH3:14]>O>[CH3:14][C:13]([C:4]1[CH:5]=[C:6]([Cl:7])[CH:1]=[CH:2][C:3]=1[Cl:8])=[O:15]

참가 물질

5

반응물 3

HCID 46851,4-DichlorobenzeneHCID 6367Acetyl chlorideHCID 6451240Aluminum(III) Chloride

생성물 1

HCID 75587Ethanone, 1-(2,5-dichlorophenyl)-

시약·촉매·용매 1

HCID 962Water용매

반응 조건

온도
110 °C

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.

후처리

  1. temperaturereflux condenser
  2. customa clear solution slowly resulting
  3. temperatureAfter cooling to room temperature
  4. customThe temperature of the mixture is kept between 30 and 40° C. during the hydrolysis by external cooling
  5. customAfter separation of the phases
  6. washthe lower, organic phase is washed with 400 ml of water
  7. customafter fresh phase separation
  8. distillationsubjected to fractional distillation

출처 및 근거

ORD 기록
ord-cc52007598bd47f7bf8ccc17a00f4812
출처 데이터셋
uspto-grants-2004_03
특허 번호
US06706930B2

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