Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Pyridine → 4-bromomethyl-2-cyclopropylmethyl-6-(3-fluoro-4-methoxyphenyl)-2H-pyridazin-3-one
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Pyridine | HCID 1049 | — |
| 반응물 | Carbon tetrabromide | HCID 11205 | — |
| 반응물 | Triphenylphosphine | HCID 11776 | — |
| 반응물 | 2-Cyclopropyl-methyl-6-(3-fluoro-4-methoxyphenyl)-4-hydroxymethyl-2H-pyridazin-3-one | HCID 67214477 | — |
| 용매 | Tetrahydrofuran | HCID 8028 | — |
| 생성물 | 4-bromomethyl-2-cyclopropylmethyl-6-(3-fluoro-4-methoxyphenyl)-2H-pyridazin-3-one | HCID 21991710 | 69.5% |
반응 단계
2-Cyclopropyl-methyl-6-(3-fluoro-4-methoxyphenyl)-4-hydroxymethyl-2H-pyridazin-3-one (185 mg, 0.61 mmol), carbon tetrabromide (404 mg, 1.2 mmol) and pyridine (48 mg, 0.61 mmol) were dissolved in tetrahydrofuran (3 mL), and under ice-cold stirring, a solution of triphenylphosphine (319 mg, 1.2 mmol) in tetrahydrofuran (3 mL) was added. Under ice cooling, the mixture was stirred for 1 hour, and further stirred overnight at room temperature. Insoluble materials were filtered off, the solvent was distilled off under reduced pressure, and the residue was isolated and purified by column chromatography on silica gel (hexane/ethyl acetate=2/1) to yield the title compound as a yellow powder (yield: 155 mg, 69.5%).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US07087606B2 |
| 출처 데이터셋 | uspto-grants-2006_08 |
| ORD ID | ord-75f5140c9d8a44fa82529fda053a0ac4 |
| 출처 메모 | uspto-grants-2006_08 |