Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Triphenylphosphine → 5-(tetrahydro-2H-pyran-4-yloxy)indan-1-one
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Triphenylphosphine | HCID 11776 | — |
| 반응물 | Tetrahydro-4H-pyran-4-ol | HCID 74956 | — |
| 반응물 | 5-Hydroxy-1-indanone | HCID 233147 | — |
| 반응물 | Dibenzyl azodicarboxylate | HCID 5387121 | — |
| 용매 | Tetrahydrofuran | HCID 8028 | — |
| 생성물 | 5-(tetrahydro-2H-pyran-4-yloxy)indan-1-one | HCID 69201344 | 85.1% |
반응 단계
5-Hydroxy-1-indanone (0.636 g, 4.30 mmol), tetrahydro-pyran-4ol (1.22 mL, 12.80 mmol), PPh3-polymer supported (2.864 g, 8.59 mmol), DBAD (1.978 g, 8.59 mmol) and THF (40 mL) were mixed, and shaken overnight. The mixture was filtered, and washed with THF (10 mL×3). The filtrate was concentrated. The residue was purified by flash chromatography to give the above intermediate (0.85 g, 85%). MS (APCI) m/z 233 (M+H)+; 1H NMR (300 MHz, CD3OD) δ ppm 1.79-1.89 (m, 2H) 2.01-2.12 (m, 2H) 2.62-2.69 (m, 2H) 3.07-3.15 (m, 2H) 3.85-4.00 (m, 4H) 4.75 (m, 1H) 6.97 (dd, J=8.65, 2.20 Hz, 1H) 7.08 (s, 1H) 7.63 (d, J=8.48 Hz, 1H).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US07320986B2 |
| 출처 데이터셋 | uspto-grants-2008_01 |
| ORD ID | ord-236c599371b04e038cd9929e46b28abb |
| 출처 메모 | uspto-grants-2008_01 |