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

HRID 49695

反応式

HRID 49695 の反応式
[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]

参加物

5

反応物 3

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 962Water溶媒

反応条件

温度
110 °C

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-cc52007598bd47f7bf8ccc17a00f4812
出典データセット
uspto-grants-2004_03
特許番号
US06706930B2

関連ノート

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