Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Monoperoxyphthalic Acid Magnesium Salt → 4-{2-[3,4-Bis(difluoromethoxy)phenyl]-2-{6-[4-(trifluoromethoxy)phenoxy]-3-pyridyl}ethyl}pyridine-N-oxide
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Monoperoxyphthalic Acid Magnesium Salt | HCID 10130449 | — |
| 반응물 | 4-{2-[3,4-Bis(difluoromethoxy)phenyl]-2-{6-[4-(trifluoromethoxy)phenoxy]-3-pyridyl}ethyl}pyridine | HCID 21262788 | — |
| 용매 | Methanol | HCID 887 | — |
| 용매 | Dichloromethane | HCID 6344 | — |
| 생성물 | 4-{2-[3,4-Bis(difluoromethoxy)phenyl]-2-{6-[4-(trifluoromethoxy)phenoxy]-3-pyridyl}ethyl}pyridine-N-oxide | HCID 21262804 | 162% |
반응 단계
To a solution of 4-{2-[3,4-bis(difluoromethoxy)phenyl]-2-{6-[4-(trifluoromethoxy)phenoxy]-3-pyridyl}ethyl}pyridine (340 mg, 0.598 mmol) from Step 5 above in a mixture of 6 mL of CH2Cl2 and 0.6 mL of MeOH, was added MMPP (222 mg, 0.359 mmol) in one portion. The mixture was stirred 24 h at room temperature and the reaction was completed with an other 50 mg of MMPP. The reaction was quenched with a saturated aqueous NaHCO3 solution and diluted with CH2Cl2. The organic layer was washed with brine, dried over MgSO4 and concentrated under reduced pressure. The residue was purified by flash chromatography on silica gel (5% MeOH/CH2Cl2) to afford the title compound as an amorphous solid (340 mg, 97%).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US06180650B2 |
| 출처 데이터셋 | uspto-grants-2001_01 |
| ORD ID | ord-ebb6f3d8ed0940de80ad1768c155f568 |
| 출처 메모 | uspto-grants-2001_01 |