関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Hexachloroethane | HCID 6214 | — |
| 反応物 | Potassium Hydroxide | HCID 14797 | — |
| 反応物 | Tetrachloroethylene | HCID 31373 | — |
| 反応物 | Montelukast Impurity 38 | HCID 12241574 | — |
| 触媒 | Dodecyltrimethylammonium chloride | HCID 8152 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | alpha,alpha,alpha,alpha'-Tetrachloroxylene | HCID 20541564 | 85.2% |
反応手順
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%.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US04966988 |
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| 出典データセット | uspto-grants-1990_10 |
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| ORD ID | ord-6580e92b726c4f0bb5b585fe2ca38b3a |
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| 出典メモ | uspto-grants-1990_10 |
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