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

HRID 1089585
ノート
印刷プレビュー

反応式

HRID 1089585 の反応式
[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
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

7

反応物 4

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

生成物 1

HCID 20541564alpha,alpha,alpha,alpha'-Tetrachloroxylene収率 85.2%

試薬・触媒・溶媒 2

HCID 8152Dodecyltrimethylammonium chloride
触媒
HCID 962Water溶媒

反応条件

温度
75 °C

実験手順

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%.

後処理

  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

出典と根拠

ORDレコード
ord-6580e92b726c4f0bb5b585fe2ca38b3a
出典データセット
uspto-grants-1990_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04966988

反応ノート

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