関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | Methanesulfonyl chloride | HCID 31297 | — |
| 反応物 | [4-(Methylsulfanyl)phenyl]methanol | HCID 592968 | — |
| 溶媒 | Toluene | HCID 1140 | — |
| 生成物 | 4-Methylthiobenzyl alcohol methanesulfonate | HCID 54323764 | 80.7% |
反応手順
In a sulfonating flask, 50 g (0.32 mol) of 4-methylthiobenzyl alcohol and 46.3 g (0.32 mol) of methylsulfonyl chloride are dissolved in 250 ml of toluene and, with cooling at 10° C., 32.5 g (0.32 mol) of triethylamine are added dropwise. The reaction mixture is then heated to room temperature and stirred overnight. 400 ml of 2N hydrochloric acid are then added to the reaction solution slowly and with cooling. The phases are separated and the organic phase is washed with water, dried over MgSO4 and concentrated in a rotary evaporator. 60 g (80%) of 4-methylthiobenzyl alcohol methanesulfonate are obtained in the form of a yellow oil.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US06017675 |
|---|
| 出典データセット | uspto-grants-2000_01 |
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| ORD ID | ord-ea819aaf204143cc9fc2fdc2d2f8d40d |
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| 出典メモ | uspto-grants-2000_01 |
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