Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Triphenylphosphine → 6,7-Dihydro-2H-pyrano[2,3-c]pyridazin-3(5H)-one
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Triphenylphosphine | HCID 11776 | — |
| 반응물 | Diisopropyl diazene-1,2-dicarboxylate | HCID 75555 | — |
| 반응물 | 4-(3-Hydroxypropyl)-1,2-dihydro-3,6-pyridazinedione | HCID 67526600 | — |
| 용매 | Tetrahydrofuran | HCID 8028 | — |
| 생성물 | 6,7-Dihydro-2H-pyrano[2,3-c]pyridazin-3(5H)-one | HCID 67526951 | 79.2% |
반응 단계
A suspension of 4-(3-hydroxypropyl)-1,2-dihydro-3,6-pyridazinedione (1.48 g, 8.7 mmol) in THF (105 ml) was held in an ultrasound bath for 5 minutes, then cooled under argon in an ice bath. Triphenylphosphine (3.67 g, 14 mmol) was added, followed by diisopropyl azodicarboxylate (2.76 ml, 14 mmol). After 30 minutes the solvent was evaporated and the residue kept under high vacuum overnight. Chromatography, eluting first with 2.5% methanol/dichloromethane until triphenylphosphine oxide was removed and then with 5% methanol/dichloromethane, gave the product as an off-white solid (1.049 g, 79%).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US07732460B2 |
| 출처 데이터셋 | uspto-grants-2010_06 |
| ORD ID | ord-742c063ba1dd404b9d9cadda52cd5a7c |
| 출처 메모 | uspto-grants-2010_06 |