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Dimethyl Sulfate → 2-(Methylthio)benzo[d]oxazol-6-ol
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Dimethyl Sulfate | HCID 6497 | — |
| 反応物 | Sodium Bicarbonate | HCID 516892 | — |
| 反応物 | HCID 178515778 | HCID 178515778 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | 2-(Methylthio)benzo[d]oxazol-6-ol | HCID 21077808 | 25.2% |
反応手順
A mixture of 6-hydroxy-2-mercaptobenzoxazole (165 mg), sodium bicarbonate (84 mg) and dimethyl sulfate (94 μl) was dissolved in water (2 ml) with stirring and under an argon atmosphere. The reaction mixture was stirred at RT overnight and HPLC showed that all starting material was gone. The reaction mixture was evaporated to dryness to give a dark brown solid (one can also extract the reaction mixture with chloroform to give the crude product). Chromatography on silica gel using 10% ethyl acetate/hexane gave the pure product as a near-white crystalline solid (45 mg, 25%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US09303026B2 |
| 出典データセット | uspto-grants-2016_04 |
| ORD ID | ord-f831a6fcb1b0468fa7c5dfa86c2d4c9d |
| 出典メモ | uspto-grants-2016_04 |