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tert-BUTYL CHLORIDE → 1,4-Dichloro-1,4-dimethylcyclohexane

HRID 1168039
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HRID 1168039 반응식
[CH3:1][CH:2]1[CH2:7][CH2:6][CH:5]([CH3:8])[CH2:4][CH2:3]1.C(Cl)(C)(C)C.[Cl-:14].[Al+3].[Cl-:16].[Cl-]>C(Cl)Cl>[Cl:14][C:2]1([CH3:1])[CH2:7][CH2:6][C:5]([Cl:16])([CH3:8])[CH2:4][CH2:3]1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 10486tert-BUTYL CHLORIDEHCID 115231,4-DimethylcyclohexaneHCID 6451240Aluminum(III) Chloride

생성물 1

HCID 124109771,4-Dichloro-1,4-dimethylcyclohexane

시약·촉매·용매 1

HCID 6344Dichloromethane용매

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온도
0 °C

실험 절차

To a solution of 1,4-dimethylcyclohexane (10 g, 89.1 mmol) and tert-butyl chloride (32.6 g, 348 mmol) in 45 mL of anhydrous methylene chloride in a 3-neck round-bottom flask under argon at 0° C., was slowly added aluminum chloride (1.24 g, 8.91 mmol). The resulting mixture was stirred at 0° C. for 1.5 hours then quenched with ice, and the product was extracted with CH2Cl2. The organic layer was separated and washed with water, and brine, and dried over Na2SO4, and filtered, and concentrated under reduced pressure. The residue was purified by Kugelrohr distillation to yield the title compound as a pale yellow liquid.

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후처리

  1. customthen quenched with ice
  2. extractionthe product was extracted with CH2Cl2
  3. customThe organic layer was separated
  4. washwashed with water, and brine
  5. dry with materialdried over Na2SO4
  6. filtrationfiltered
  7. concentrationconcentrated under reduced pressure
  8. distillationThe residue was purified by Kugelrohr distillation

출처 및 근거

ORD 기록
ord-6d3a31de85e4466880da3563e5145a1e
출처 데이터셋
uspto-grants-2003_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06620963B1

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