Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Sodium Hydroxide → 5-Bromopyridine-2-carbonitrile
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Sodium Hydroxide | HCID 14798 | — |
| 반응물 | Phosphorus oxychloride | HCID 24813 | — |
| 반응물 | 5-Bromopyridine-2-carboxamide | HCID 735151 | — |
| 용매 | Toluene | HCID 1140 | — |
| 생성물 | 5-Bromopyridine-2-carbonitrile | HCID 817154 | 82.7% |
반응 단계
Phosphorus oxychloride (111 g, 0.720 mol) was added to a mixture of 5-bromopicolinamide (D8) (58 g, 0.288 mol) in dry toluene (300 ml) The mixture was heated to reflux for 2 hours. The mixture was poured into ice/water, and basified to pH=12 with 2N NaOH. The resulting mixture was extracted with ethyl acetate and the organic phase was washed with brine, dried over Na2SO4, and concentrated in vacuo. The residue was purified by column chromatography on silica gel eluting with a mixture petroleum ether/ethyl acetate 10:1. Collected fractions, after solvent evaporation afforded the title compound (D9) (43.6 g) as a yellow solid.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US08828987B2 |
| 출처 데이터셋 | uspto-grants-2014_09 |
| ORD ID | ord-e83cf6404d21478aac0b005324c1ef0e |
| 출처 메모 | uspto-grants-2014_09 |