Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Pyridine → methyl 4-(3-bromo-4-fluorophenyl)-2-(bromomethyl)-5-oxo-4,5,6,8-tetrahydro-1H-pyrano[3,4-b]pyridine-3-carboxylate
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Pyridine | HCID 1049 | — |
| 반응물 | methyl 4-(3-bromo-4-fluorophenyl)-2-methyl-5-oxo-4,5,6,8-tetrahydro-1H-pyrano[3,4-b]pyridine-3-carboxylate | HCID 11257964 | — |
| 반응물 | Pyridiniumtribromide | HCID 21124087 | — |
| 용매 | Chloroform | HCID 6212 | — |
| 용매 | Dichloromethane | HCID 6344 | — |
| 생성물 | methyl 4-(3-bromo-4-fluorophenyl)-2-(bromomethyl)-5-oxo-4,5,6,8-tetrahydro-1H-pyrano[3,4-b]pyridine-3-carboxylate | HCID 11328992 | 65.1% |
반응 단계
A solution of the product from Example 25A (0.87 g, 2.2 mmol) in chloroform (10 mL) was cooled to −10° C., treated with pyridine (0.21 mL, 2.6 mmol), then treated with pyridinium tribromide (0.84 g, 2.6 mmol), stirred for 1 hour, diluted with methylene chloride (150 mL) and washed with 1N HCl (25 mL). The organic layer was dried (MgSO4), filtered and concentrated. The residue was purified by flash chromatography over silica gel (1% and then 2% methanol/methylene chloride) to provide the title compound (0.68 g) as an oil.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US06642222B2 |
| 출처 데이터셋 | uspto-grants-2003_11 |
| ORD ID | ord-8bed5de56ee3472aa75fd3a2d2caa963 |
| 출처 메모 | uspto-grants-2003_11 |