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Hexachloroethane → alpha,alpha,alpha,alpha'-Tetrachloroxylene

HRID 1089585
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HRID 1089585 반응식
[Cl:1][CH:2](Cl)[C:3]1C=[CH:7][CH:6]=[C:5](CCl)[CH:4]=1.ClC(Cl)=C(Cl)Cl.[Cl:18][C:19]([Cl:25])([Cl:24])[C:20](Cl)(Cl)Cl.[OH-].[K+]>[Cl-].C([N+](C)(C)C)CCCCCCCCCCC.O>[Cl:18][C:19]([Cl:25])([Cl:24])[C:20]1[C:3]([CH2:2][Cl:1])=[CH:4][CH:5]=[CH:6][CH:7]=1
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참가 물질

7

반응물 4

HCID 6214HexachloroethaneHCID 14797Potassium HydroxideHCID 31373TetrachloroethyleneHCID 12241574Montelukast Impurity 38

생성물 1

HCID 20541564alpha,alpha,alpha,alpha'-Tetrachloroxylene수율 85.2%

시약·촉매·용매 2

HCID 8152
Dodecyltrimethylammonium chloride
촉매
HCID 962Water용매

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온도
75 °C

실험 절차

α,α,α'-Trichloro-m-xylene (22.5 grams, 93.2% a.i., 0.1 moles) was dissolved in 18 mls. of tetrachloroethylene. Hexachloroethane (59.2 grams, 0.25 moles), potassium hydroxide (12.8 grams, 87.7%, 0.2 moles), water (2.13 grams), and dodecyltrimethylammonium chloride (0.255 grams, 0.001 moles) were added. The mixture was heated at 75° C. for 2.5 hours with good stirring. The reaction was quenched with 30 mls. of water and 18 mls tetrachloroethylene. The organic phase was separated and washed with water. The excess solvent and hexachloroethane were distilled off to give an 85.2% yield of α,α,α,α'-tetrachloroxylene with a purity of 84%.

후처리

  1. dissolution, 0.1 moles) was dissolved in 18 mls
  2. customThe reaction was quenched with 30 mls
  3. customThe organic phase was separated
  4. washwashed with water
  5. distillationThe excess solvent and hexachloroethane were distilled off

출처 및 근거

ORD 기록
ord-6580e92b726c4f0bb5b585fe2ca38b3a
출처 데이터셋
uspto-grants-1990_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04966988

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