참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | 3,5-Dichlorobenzoic acid | HCID 5811 | — |
| 반응물 | Triethylamine | HCID 8471 | — |
| 반응물 | Isobutyl chloroformate | HCID 62365 | — |
| 반응물 | N-Methylhydrazinecarbothioamide | HCID 2723853 | — |
| 용매 | Tetrahydrofuran | HCID 8028 | — |
| 생성물 | HCID 178462985 | HCID 178462985 | 8.5% |
반응 단계
3,5-Dichloro-benzoic acid (382 mg, 2 mmol) was mixed with triethylamine (606 mg, 3 mmol) in THF (6 ml) at 10° C. Then isobutyl chloroformate (300 mg, 2.2 mmol) was added dropwise and stirred for 45 min. To the reaction mixture, 4-methyl-3-thiosemicarbazide (238.4 mg, 2 mmol) was added. After being stirred at room temperature for 10 min, the reaction mixture was heated to 70° C. overnight. Standard work-up. The product was purified by column chromatography with 25˜30% ethyl acetate in hexanes to give 46.4 mg (8.5%) of 5-(3,5-dichloro-phenyl)-4-ethyl-4H-[1,2,4]triazole-3-thiol.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US07456200B2 |
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| 출처 데이터셋 | uspto-grants-2008_11 |
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| ORD ID | ord-e822db12a34d4ad296bf027c2f54e953 |
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| 출처 메모 | uspto-grants-2008_11 |
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