関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Methanesulfonic Acid | HCID 6395 | — |
| 反応物 | 2-Methylbenzenesulfonic acid | HCID 6925 | — |
| 反応物 | Phosphorus oxide (P4O10) | HCID 14812 | — |
| 反応物 | 3,4-Dimethoxytoluene | HCID 68126 | — |
| 生成物 | 1,2-Dimethoxy-4-(2-methylphenylsulphonyl)-5-methylbenzene | HCID 23312101 | — |
反応手順
50 g of phosphorus pentoxide are covered, by pouring, with 400 ml of methanesulphonic acid and the whole is stirred at 60° until a clear solution has formed. 30.4 g (0.2 mol) of 1,2-dimethoxy-4-methylbenzene and 43 g (0.2 mol) of 2-methylbenzenesulphonic acid (80% strength) are then added, and the internal temperature is increased to 80° for 30 minutes. The mixture is poured onto 4 liters of ice-water and extracted with ethyl acetate. The extract solution is washed twice with water, dried over sodium sulphate, filtered and concentrated by evaporation in a rotary evaporator. The oil remaining crystallises immediately. It is triturated with diethyl ether and filtered off. In this manner colourless crystals of 1,2-dimethoxy-4-(2-methylphenylsulphonyl)-5-methylbenzene having a melting point of 126°-128° are obtained.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US04600709 |
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| 出典データセット | uspto-grants-1986_07 |
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| ORD ID | ord-185eac5d815741e5845b015b06bc3790 |
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| 出典メモ | uspto-grants-1986_07 |
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