関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Triethyl orthoacetate | HCID 66221 | — |
| 反応物 | m-Bromobenzohydrazide | HCID 520941 | — |
| 溶媒 | Acetic Acid | HCID 176 | — |
| 生成物 | 2-(3-Bromophenyl)-5-methyl-1,3,4-oxadiazole | HCID 26966989 | 35% |
反応手順
In a pressure vessel was suspended 3-bromobenzohydrazide (1.8 g, 8.37 mmol) in 14 ml acetic acid. 1,1,1-Triethoxyethane (4.6 ml, 25 mmol) was added and the reaction was stirred at 150° C. for 3 h. The solvent was concentrated under reduced pressure and the crude was washed with sodium bicarbonate and brine. The organic layer was dried over sodium sulphate, filtered and evaporated under reduced pressure. The residue was re-dissolved in dichloromethane, concentrated under reduced pressure and a solid was precipitated. This solid was washed with diethylether, filtered and dried in the vacuum oven at 40° C. to obtain 670 mg (35% yield) of the title compound. Purity 100%.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US09388189B2 |
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| 出典データセット | uspto-grants-2016_07 |
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| ORD ID | ord-6c0c18c9922b4f81b5e7fe664a813112 |
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| 出典メモ | uspto-grants-2016_07 |
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