Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Hydrogen Peroxide → 5-(2-Methylsulfonylpyrimidin-4-yl)-6-(3-trifluoromethylphenyl)-4,5-dihydro-2H-pyridazin-3-one
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Hydrogen Peroxide | HCID 784 | — |
| 반응물 | Methanol | HCID 887 | — |
| 반응물 | Sodium Dithionite | HCID 24489 | — |
| 반응물 | 5-(2-Methylsulfanylpyrimidin-4-yl)-6-(3-trifluoromethylphenyl)-4,5-dihydro-2H-pyridazin-3-one | HCID 18176626 | — |
| 촉매 | Sodium tungstate | HCID 26052 | — |
| 용매 | Ethyl Acetate | HCID 8857 | — |
| 생성물 | 5-(2-Methylsulfonylpyrimidin-4-yl)-6-(3-trifluoromethylphenyl)-4,5-dihydro-2H-pyridazin-3-one | HCID 18176613 | — |
반응 단계
Compound 6 (17.8 mmol), sodium tungstate (587 mg, 1.78 mmol), 30% hydrogen peroxide (8.07 mL, 71.2 mmol), methanol (20 mL), and ethyl acetate (200 mL) were combined under argon, then heated to reflux for 4 h. The solution was cooled and aqueous sodium hydrosulfite was added. The methanol was removed in vacuo and saturated sodium bicarbonate was added. The resulting suspension was extracted several times with methylene chloride. The combined organic extracts were washed successively with water and brine. The organic layer was dried with anhydrous sodium sulfate then concentrated in vacuo to give Compound 7 as a foam: 5.0 g (13 mmol, 73% (two steps))
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US06602872B1 |
| 출처 데이터셋 | uspto-grants-2003_08 |
| ORD ID | ord-c0547385b9c942c6ba5de8f00893f129 |
| 출처 메모 | uspto-grants-2003_08 |