Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Water → Benzyl 4-(2-(1-bromo-2,2,2-trifluoroethylidene)hydrazinyl)piperidine-1-carboxylate
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Water | HCID 962 | — |
| 반응물 | Ethyl Acetate | HCID 8857 | — |
| 반응물 | N-bromobutanimide | HCID 67184 | — |
| 반응물 | Benzyl 4-(2-(2,2,2-trifluoroethylidene)hydrazinyl)piperidine-1-carboxylate | HCID 69095121 | — |
| 용매 | Dimethylformamide | HCID 6228 | — |
| 용매 | Sodium chloride; water | HCID 57417360 | — |
| 생성물 | Benzyl 4-(2-(1-bromo-2,2,2-trifluoroethylidene)hydrazinyl)piperidine-1-carboxylate | HCID 72576664 | 47.2% |
반응 단계
To a stirred solution of 110 (2.881 g, 8.75 mmol) in DMF (29.2 ml) was added NBS (1.713 g, 9.62 mmol) and the resulting solution was allowed to stir for 1 h at room temperature. Ethyl acetate was added followed by brine and water (50/50), and the AcOEt extracts were washed with water and brine, dried over MgSO4, filtrated and concentrated. The residue was purified via Biotage (5% to 20% EtOAc/Hexane; 25M column) to afford 111 (1.685 g, 47.2% yield) as yellow oil. LRMS (ESI): calc. 407.05 and 409.04; found 408.2 and 410.2 (MH)+.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US08338437B2 |
| 출처 데이터셋 | uspto-grants-2012_12 |
| ORD ID | ord-1cfab658b86b4bb48a29122423ec33cc |
| 출처 메모 | uspto-grants-2012_12 |