참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Dimethylformamide dimethyl acetal | HCID 78373 | — |
| 반응물 | 4-Bromo-2-fluorobenzamide | HCID 2773331 | — |
| 생성물 | HCID 178484324 | HCID 178484324 | 96% |
반응 단계
A suspension of 4-bromo-2-fluorobenzamide (0.929 g, 4.26 mmol) in 1,1-dimethoxy-N,N-dimethylmethanamine (1.66 mL, 11.7 mmol) in a round bottom flask topped with a short path distillation head was heated to 100-100° C. The resulting solution was allowed to stir at this temperature for 3.5 hours, during which time the MeOH that was formed was collected from the distillation condenser. Heptane (5 mL) was added dropwise and the resulting suspension was cooled to 0-5° C. The solids were collected by vacuum filtration, rinsed with excess heptane, and dried to afford (E)-4-bromo-N-((dimethylamino)methylene)-2-fluorobenzamide (1.111 g, 96%) as an off-white solid which was carried on without further purification.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US08865726B2 |
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| 출처 데이터셋 | uspto-grants-2014_10 |
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| ORD ID | ord-e7785fe88bcf49729865d73fc3f9046e |
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| 출처 메모 | uspto-grants-2014_10 |
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