Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Dimethylformamide → 3-(1-{[2-Bromo-3',5'-bis(trifluoromethyl)biphenyl-4-yl]carbonyl}pyrrolidin-3-yl)pyridine
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Dimethylformamide | HCID 6228 | — |
| 반응물 | 1-Hydroxybenzotriazole | HCID 75771 | — |
| 반응물 | 1,3-Propanediamine, N'-(ethylcarbonimidoyl)-N,N-dimethyl-, monohydrochloride | HCID 2723939 | — |
| 반응물 | 2-Bromo-3',5'-bis(trifluoromethyl)biphenyl-4-carboxylic acid | HCID 86657756 | — |
| 생성물 | 3-(1-{[2-Bromo-3',5'-bis(trifluoromethyl)biphenyl-4-yl]carbonyl}pyrrolidin-3-yl)pyridine | HCID 86657753 | — |
반응 단계
i-5d (179 mg, 1.21 mmol) was added to a stirred solution of 3a (500 mg, 1.21 mmol), N-(3-dimethylaminopropyl)-N-ethylcarbodiimide hydrochloride (255 mg, 1.33 mmol) and 1-hydroxybenzotriazole 185 mg, 1.21 mmol) in DMF (8.00 mL). After 4 h, the reaction mixture was quenched with said, aq. NaHCO3 and extracted with EtOAc. The organic layer was washed with water and brine, dried (sodium sulfate) and concentrated in vacuo. The resulting crude residue was purified by column chromatography on silica gel (gradient elution; 0%-5% methanol/EtOAc as eluent) to afford the title compound 3b. m/z (ES) 543 (MH)+.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US08367679B2 |
| 출처 데이터셋 | uspto-grants-2013_02 |
| ORD ID | ord-565eb4acbea748179c320f971fd30d70 |
| 출처 메모 | uspto-grants-2013_02 |