참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Triethylamine | HCID 8471 | — |
| 반응물 | Hydrazinecarboxaldehyde | HCID 12229 | — |
| 반응물 | Ethyl 4-bromobenzimidate hydrochloride | HCID 19017302 | — |
| 생성물 | HCID 178419362 | HCID 178419362 | 48.3% |
반응 단계
Ethyl 4-bromobenzimidate hydrochloride (35.6 g, 135 mmol), formic hydrazide (16.16 g, 269 mmol) and triethylamine (75 mL, 538 mmol) were combined in a screw capped flask and heated to 85° C. for 16 h. The solution was condensed under reduced pressure to afford a solid, which was partitioned between water and ethyl acetate (3×), dried over magnesium sulfate and solvent removed under reduced pressure. The resulting solid was sonicated with 20% ethyl acetate in hexanes, filtered and dried to afford the title compound (14.6 g, 65.2 mmol, 48% yield). MS (ESI) m/z 224.1 [M]+, 226.1 [M+2]+.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US08907087B2 |
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| 출처 데이터셋 | uspto-grants-2014_12 |
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| ORD ID | ord-a4dc0992baba4b5aa14cfd7a0216fe56 |
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| 출처 메모 | uspto-grants-2014_12 |
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