Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Triphenylphosphine → 3-{4-[3-(4-Ethoxylphenoxy)propyl]piperazin-1-yl}-6-chloropyridazine
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Triphenylphosphine | HCID 11776 | — |
| 반응물 | 4-Ethoxyphenol | HCID 12150 | — |
| 반응물 | Diethyl azodicarboxylate | HCID 5462977 | — |
| 반응물 | 3-[4-(6-Chloropyridazin-3-yl)piperazin-1-yl]propan-1-ol | HCID 86762798 | — |
| 용매 | Tetrahydrofuran | HCID 8028 | — |
| 생성물 | 3-{4-[3-(4-Ethoxylphenoxy)propyl]piperazin-1-yl}-6-chloropyridazine | HCID 51003562 | 23.9% |
반응 단계
3-[4-(6-chloropyridazin-3-yl)piperazin-1-yl]propan-1-ol (0.77 g, 3 mmol), p-ethoxylphenol (0.41 g, 3 mmol), triphenylphosphine (0.79 g, 3 mmol) and anhydrous THF (20 mL) were placed in a 100 mL three-necked bottle, and DEAD (0.52 g, 3 mmol) was added slowly in dropwise within 10 min under an ice-bath condition. The mixture was stirred at room temperature overnight, subjected to a column chromatography (eluting agent: petroleum/ethyl acetate, v/v 3: 2) to obtain a white solid, 0.27 g, yield 23.9%. mp: 125-127° C.; 1H-NMR (400 MHz, CDCl3, δppm) δ1.39(t, 3H, J=7.2 Hz), 2.00(m, 2H), 2.61(br, 6H), 3.67(br, 4H), 3.98 (m, 4H), 6.83(s, 4H), 6.90(d, 1H, J=9.6 Hz), 7.21(d, 1H, J=9.6 Hz); EI-MS(m/z): 376.2[M+H].
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US08846678B2 |
| 출처 데이터셋 | uspto-grants-2014_09 |
| ORD ID | ord-e3f47881de454df681c920a9ccaf3483 |
| 출처 메모 | uspto-grants-2014_09 |