関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Carbon Tetrachloride | HCID 5943 | — |
| 反応物 | 1,3-Diisopropylbenzene | HCID 7450 | — |
| 反応物 | Chloromethyl ethyl ether | HCID 18523 | — |
| 反応物 | Tin tetrachloride | HCID 24287 | — |
| 生成物 | 1,5-Bis(chloromethyl)-2,4-di(propan-2-yl)benzene | HCID 14850543 | — |
反応手順
55 ml (0.46 mol) of tin tetrachloride are added dropwise with cooling in an ice bath (exothermic reaction) to a solution of 230 ml (2.43 mol) of chloromethyl ethyl ether and 197 g (1.22 mol) of 1,3-diisopropylbenzene in 600 ml of carbon tetrachloride and the mixture is stirred at 0° C. for 1 h. After stirring overnight at +25° C., 142 g (1.5 mol) of chloromethyl ethyl ether and 74 ml (0.46 mol) of tin tetrachloride are again added dropwise at 0° C. and the mixture is stirred overnight at +25° C. The reaction mixture is added to ice/hydrochloric acid, and the organic phase is separated off, washed with water and dried using sodium sulphate. After concentrating, the residue is taken up with petroleum ether, filtered through 1 kg of silica gel (230-400 mesh) and distilled in a high vacuum.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US05138090 |
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| 出典データセット | uspto-grants-1992_08 |
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| ORD ID | ord-1b88865d09304a0d95c270c7508e6ee6 |
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| 出典メモ | uspto-grants-1992_08 |
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