Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Dichloromethane → 3-Methyl-5-nitro-2-phenylpyridine
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Dichloromethane | HCID 6344 | — |
| 반응물 | Cesium carbonate | HCID 10796 | — |
| 반응물 | Phenylboronic Acid | HCID 66827 | — |
| 반응물 | 2-Bromo-3-methyl-5-nitropyridine | HCID 5200466 | — |
| 용매 | 1,4-Dioxane--water (1/1) | HCID 21886435 | — |
| 생성물 | 3-Methyl-5-nitro-2-phenylpyridine | HCID 46315057 | 97% |
반응 단계
In a schlenck tube, a mixture of 2-bromo-3-methyl-5-nitropyridine (4.6 mmol, 1.0 g), phenylboronic acid (4.6 mmol, 0.560 g), PdCl2dppf.DCM (0.47 mmol, 0.4 g), Cs2CO3 (13.8 mmol, 4.5 g) in a dioxane/water 4:1 mixture (18 ml) was heated at 100° C. for 14 hours, under argon atmosphere. The solvent was evaporated and the crude mixture was extracted between water and ethyl acetate. The solid residue was purified by chromatography over SiO2 eluting with hexane/ethyl acetate mixtures affording 3-methyl-5-nitro-2-phenylpyridine (0.95 g, yield 97%) as major product.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US08536165B2 |
| 출처 데이터셋 | uspto-grants-2013_09 |
| ORD ID | ord-6712a36184ac4dfaa445b8e584cf2b21 |
| 출처 메모 | uspto-grants-2013_09 |