Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Sodium Carbonate → 6-[(R)-4-(4-Benzylphthalazin-1-yl)-2-methylpiperazin-1-yl]nicotinonitrile
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Sodium Carbonate | HCID 10340 | — |
| 반응물 | 6-Chloro-3-pyridinecarbonitrile | HCID 5152094 | — |
| 반응물 | 1-Benzyl-4-((R)-3-methyl-piperazin-1-yl)-phthalazine | HCID 44186248 | — |
| 용매 | Dimethylformamide | HCID 6228 | — |
| 용매 | 1,4-Dioxane | HCID 31275 | — |
| 생성물 | 6-[(R)-4-(4-Benzylphthalazin-1-yl)-2-methylpiperazin-1-yl]nicotinonitrile | HCID 44186480 | 42.2% |
반응 단계
Solid Na2CO3 (50 mg, 0.47 mmol, 1.5 eq) is added to a solution of 6-chloronicotinonitrile (50 mg, 0.36 mmol, 1.2 eq), 1-benzyl-4-((R)-3-methyl-piperazin-1-yl)-phthalazine (100 mg, 0.31 mmol, 1.0 eq) in DMF (1 mL) and dioxane (2 mL) in a microwave vial. The vial is sealed and irradiated in the microwave at 180° C. (high absorption setting) for 30 minutes. The reaction mixture is concentrated, dichloromethane is added and is washed with water then brine. The organic fraction is dried over sodium sulfate, and is evaporated under reduced pressure, then purified by flash chromatography (50%-90% EtOAc/Hexane) to afford the title compound as a white solid (55 mg, 42% yield).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US08536168B2 |
| 출처 데이터셋 | uspto-grants-2013_09 |
| ORD ID | ord-0ba5931c41c24e159e704285350d2dc6 |
| 출처 메모 | uspto-grants-2013_09 |