Hydrochloric Acid → 1,4-Dichloro-2-cyclohexylbenzene

HRID 1164520

反応式

HRID 1164520 の反応式
[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([Cl:8])=[CH:4][CH:3]=1.[Cl-].[Al+3].[Cl-].[Cl-].Cl[CH:14]1[CH2:19][CH2:18][CH2:17][CH2:16][CH2:15]1.Cl>C(=S)=S>[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([Cl:8])=[CH:4][C:3]=1[CH:14]1[CH2:19][CH2:18][CH2:17][CH2:16][CH2:15]1

参加物

6

反応物 4

HCID 313Hydrochloric AcidHCID 46851,4-DichlorobenzeneHCID 10952ChlorocyclohexaneHCID 6451240Aluminum(III) Chloride

生成物 1

HCID 130971441,4-Dichloro-2-cyclohexylbenzene収率 25.3%

試薬・触媒・溶媒 1

HCID 6348Carbon Disulfide溶媒

実験手順

To a solution of 1,4-dichlorobenzene (294 g) in anhydrous carbon disulfide (400 ml) was added anhydrous aluminum chloride (16.0 g). To the mixture was added dropwise chlorocyclohexane (96 g) with stirring at ambient temperature during 3 hours. After the stirring was continued for 3 hours at ambient temperature, the reaction mixture was allowed to stand overnight at ambient temperature. To the reaction mixture was added dil.hydrochloric acid with stirring. The organic layer was separated, washed with water, dried over magnesium sulfate, concentrated under reduced pressure and allowed to stand at ambient temperature for a while to give precipitates. The precipitates were removed by filtration. The filtrate was distilled under reduced pressure to give 1,4-dichloro-2-cyclohexylbenzene (47.0 g).

後処理

  1. waitAfter the stirring was continued for 3 hours at ambient temperature
  2. waitto stand overnight at ambient temperature
  3. additionTo the reaction mixture was added dil
  4. customThe organic layer was separated
  5. washwashed with water
  6. dry with materialdried over magnesium sulfate
  7. concentrationconcentrated under reduced pressure
  8. customto stand at ambient temperature for a while
  9. customto give
  10. customprecipitates
  11. customThe precipitates were removed by filtration
  12. distillationThe filtrate was distilled under reduced pressure

出典と根拠

ORDレコード
ord-81343abefe244d0cab64d765d06a5af8
出典データセット
uspto-grants-1983_01
特許番号
US04370340

関連ノート

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