関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | o-Toluenesulfonyl chloride | HCID 8623 | — |
| 反応物 | Methyl Glycolate | HCID 66774 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | Methyl toluenesulfonyloxyacetate | HCID 86751745 | 98.3% |
反応手順
18 g (0.2 mol) of methyl hydroxyacetate and 20.2 g (0.2 mol) of triethylamine are first introduced into 300 ml of dichloromethane at 0° C. 41.9 g (0.22 mol) of toluenesulfonyl chloride are then added at this temperature in small portions. Stirring of the batch at 0° C. is continued overnight. Ice water is added, the phases are separated, and the aqueous phase is extracted three times with dichloromethane. The combined organic phases are washed once with water, dried, and the solvent is removed on a rotary evaporator. 48 g (98% of theory) of methyl toluenesulfonyloxyacetate having a GC content of 96% are isolated as a colorless solid.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US05698735 |
|---|
| 出典データセット | uspto-grants-1997_12 |
|---|
| ORD ID | ord-49cbc3da55944ccc97d427074c032aa5 |
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| 出典メモ | uspto-grants-1997_12 |
|---|
