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Dimethyl Sulfate → 2-Methylthio-1,3-dithiolium perchlorate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Dimethyl Sulfate | HCID 6497 | — |
| 反応物 | 1,3-Dithiole-2-Thione | HCID 70254 | — |
| 反応物 | Sodium Perchlorate | HCID 522606 | — |
| 生成物 | 2-Methylthio-1,3-dithiolium perchlorate | HCID 23039009 | 85.8% |
反応手順
A mixture comprising 26.8g (0.2 mole) of 1,3-dithiol-2-thion and 25.2g (0.2 mole) of dimethylsulfuric acid was reacted at 60° C for 30 minutes and then at 90° C for 30 minutes. After cooling, the reaction product was poured into 150 ml of a saturated aqueous sodium perchlorate solution to deposit crystals. The crystals were recovered by filtration, washed with ether, dried and then recrystallized from methanol to obtain 42.5g of yellow crystals, m.p. 42°-46° C, yield 85.8%.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04035387 |
| 出典データセット | uspto-grants-1977_07 |
| ORD ID | ord-8343701e29dc4a75aa09243617e9cd4b |
| 出典メモ | uspto-grants-1977_07 |