関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | Phosphorus tribromide | HCID 24614 | — |
| 反応物 | [3-(4-Benzyloxyphenyl)-[1,2,4]thiadiazol-5-yl]-methanol | HCID 59549522 | — |
| 溶媒 | Toluene | HCID 1140 | — |
| 生成物 | 3-(4-Benzyloxyphenyl)-5-bromomethyl-[1,2,4]thiadiazole | HCID 59549527 | 70% |
反応手順
To a solution of [3-(4-benzyloxyphenyl)-[1,2,4]thiadiazol-5-yl]-methanol (0.052 g, 0.17 mmol) in toluene (5 ml) was added PBr3 (0.027 ml, 0.26 mmol) and the resulting reaction mixture was refluxed at 120° C. for 15 min. After the completion of the reaction (TLC monitoring), the reaction mixture was cooled to 0° C., added water (50 ml) and extracted with ethyl acetate (3×50 ml). The combined organics was washed with saturated NaHCO3 solution, dried over Na2SO4, filtered and concentrated under vacuum to get the desired product (0.043 g, 68%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08492414B2 |
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| 出典データセット | uspto-grants-2013_07 |
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| ORD ID | ord-33aa0356b7c5406e8ec4fe009113d37b |
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| 出典メモ | uspto-grants-2013_07 |
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