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Methyl iodide → 3-methylthio-11H-s-triazolo[3,4-b][3]benzazepine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Methyl iodide | HCID 6328 | — |
| 反応物 | 2,11-dihydro-3H-s-triazolo[3,4-b][3]benzazepine-3-thione | HCID 13072423 | — |
| 反応物 | Sodium methanolate methanol | HCID 23694274 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 生成物 | 3-methylthio-11H-s-triazolo[3,4-b][3]benzazepine | HCID 21323406 | — |
反応手順
To 3 ml of methanol was added 0.215 g of 2,11-dihydro-3H-s-triazolo[3,4-b][3]benzazepine-3-thione and, under stirring, 0.6 ml of 2N-sodium methoxide/methanol was added. Then, 0.07 ml of methyl iodide was added dropwise. After 20 minutes, the reaction mixture was extracted with ethyl acetate. The ethyl acetate layer was washed with water and dried over Na2SO4. The solvent was then evaporated off and the residue was treated with ether. In this manner, 3-methylthio-11H-s-triazolo[3,4-b][3]benzazepine were obtained as crystals. Recrystallization from methanol yielded colorless needles melting at 168°-169° C. This was identical with the products obtained in Examples 1 and 2.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04150139 |
| 出典データセット | uspto-grants-1979_04 |
| ORD ID | ord-bab0281336fd44af883de71d8461ae1f |
| 出典メモ | uspto-grants-1979_04 |