Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Dichloromethane → 2-(3,5-Bis-(4-fluoro-phenyl)-(1,2,4)triazol-1-yl)-1-(4-(5-methoxy-pyrimidin-2-yl)-piperazin-1-yl)-ethanone
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Dichloromethane | HCID 6344 | — |
| 반응물 | Diisopropylethylamine | HCID 81531 | — |
| 반응물 | (3,5-bis-(4-Fluoro-phenyl)-(1,2,4)triazol-1-yl)-acetic acid | HCID 86686517 | — |
| 반응물 | 5-Methoxy-2-piperazin-1-yl-pyrimidine hydrochloride | HCID 86686609 | — |
| 용매 | Dimethylformamide | HCID 6228 | — |
| 생성물 | 2-(3,5-Bis-(4-fluoro-phenyl)-(1,2,4)triazol-1-yl)-1-(4-(5-methoxy-pyrimidin-2-yl)-piperazin-1-yl)-ethanone | HCID 71666564 | 20.5% |
반응 단계
100 mg (3,5-bis-(4-fluoro-phenyl)-(1,2,4)triazol-1-yl)-acetic acid was dissolved in 2 mL DMF. 163 mg PFTU and 0.5 mL DIPEA were added to this solution and the mixture was stirred for 7 min at RT. Then, 88 mg 5-Methoxy-2-piperazin-1-yl-pyrimidine hydrochloride and 0.11 mL DIPEA dissolved in 1.5 mL DMF were added and the reaction was stirred 3 h at RT. Then, a saturated sodiumhydrogencarbonate solution and CH2Cl2 were added, the organic phase was separated and the solvent was removed. The residue was purified by HPLC and crystallized with diethylether to give 32 mg of the desired compound. Rt: 0.82 min (method E), (M+H)+: 492
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US08889677B2 |
| 출처 데이터셋 | uspto-grants-2014_11 |
| ORD ID | ord-17e437f69b6c4c68b4d9eb90bdbaf8d1 |
| 출처 메모 | uspto-grants-2014_11 |