Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Sodium Carbonate → 4-(1-methylpiperidin-4-yloxy)-2-phenyl-9,10-dihydro-4H-3,10a-diaza-benzo[f]azulene
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Sodium Carbonate | HCID 10340 | — |
| 반응물 | 4-Piperidinol, 1-methyl- | HCID 66048 | — |
| 반응물 | 1-Phenethyl-4-phenyl-imidazole-2-carbaldehyde | HCID 86703947 | — |
| 용매 | Chloroform | HCID 6212 | — |
| 용매 | Methanesulfonic Acid | HCID 6395 | — |
| 생성물 | 4-(1-methylpiperidin-4-yloxy)-2-phenyl-9,10-dihydro-4H-3,10a-diaza-benzo[f]azulene | HCID 72695779 | — |
반응 단계
To a solution of 4-hydroxy-N-methylpiperidine (275 mg, 2.39 mmoles) in methanesulfonic acid (2 mL) at 0° C. is added a solution of 1-phenethyl-4-phenyl-imidazole-2-carbaldehyde (example 4B) (250 mg, 0.904 mmoles) in chloroform (2 mL). The reaction mixture is stirred at room temperature overnight, then heated to reflux for 6 h. A saturated solution of Na2CO3 is added to reach pH 10. The aqueous phase is extracted three times with CH2Cl2. The organic phase is dried over magnesium sulphate, filtered and the solvent is removed under reduced pressure. The residue is purified by silica gel chromatography using (CH2Cl2:MeOH) (90:10) to give 4-(1-methylpiperidin-4-yloxy)-2-phenyl-9,10-dihydro-4H-3,10a-diaza-benzo[f]azulene melting at 113° C.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US09255101B2 |
| 출처 데이터셋 | uspto-grants-2016_02 |
| ORD ID | ord-a98f6ab652fb447c90e4a58ed8cc0356 |
| 출처 메모 | uspto-grants-2016_02 |