참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Triethyl orthoacetate | HCID 66221 | — |
| 반응물 | m-Bromobenzohydrazide | HCID 520941 | — |
| 용매 | Acetic Acid | HCID 176 | — |
| 생성물 | 2-(3-Bromophenyl)-5-methyl-1,3,4-oxadiazole | HCID 26966989 | 35% |
반응 단계
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%.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US09388189B2 |
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| 출처 데이터셋 | uspto-grants-2016_07 |
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| ORD ID | ord-6c0c18c9922b4f81b5e7fe664a813112 |
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| 출처 메모 | uspto-grants-2016_07 |
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