참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Hydrazine hydrate (1:1) | HCID 24654 | — |
| 반응물 | Dimethylformamide dimethyl acetal | HCID 78373 | — |
| 반응물 | 4-Bromo-2-fluorobenzamide | HCID 2773331 | — |
| 용매 | Acetic Acid | HCID 176 | — |
| 생성물 | HCID 178505414 | HCID 178505414 | 68.1% |
반응 단계
4-Bromo-2-fluorobenzamide (9.53 g, 43.7 mmol) and N,N-dimethylformamide dimethylacetal (75.0 mL) were combined in a 500 mL round bottom flask and purged with nitrogen. The reaction was heated to reflux at 85° C. for 2 h. The resulting mixture was concentrated under reduced pressure and dried under vacuum to afford a yellow oil. The oil was suspended in concentrated acetic acid (75.0 mL) and cooled to 0° C. Hydrazine hydrate (21.88 g, 437 mmol) was added dropwise and the mixture was allowed to stir at rt for 5 h. The reaction was poured warm onto cold ice and extracted with dichloromethane (3×200 mL). Organic volatiles were removed under reduced pressure to afford 3-(4-bromo-2-fluorophenyl)-4H-1,2,4-triazole (7.20 g, 29.7 mmol, 68.1% yield) as a white solid. MS (ESI) m/z 241.9 [M]+, 243.9 [M+2]+.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US09193692B2 |
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| 출처 데이터셋 | uspto-grants-2015_11 |
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| ORD ID | ord-fda8fa588132452f8a3977c5c7be6d01 |
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| 출처 메모 | uspto-grants-2015_11 |
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