Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Phosphorus trichloride → 4-bromo-2,2'-bipyridine
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Phosphorus trichloride | HCID 24387 | — |
| 반응물 | 4-Bromo-1-oxo-2-(pyridin-2-yl)-1lambda~5~-pyridine | HCID 18172778 | — |
| 용매 | Chloroform | HCID 6212 | — |
| 생성물 | 4-bromo-2,2'-bipyridine | HCID 12087122 | 85% |
반응 단계
To a stirred suspension of 4-bromo-2,2′-bipyridyl-N-oxide in 60 mL CHCl3, was added 12 mL PCl3, at room temperature. The mixture was refluxed for 2 h under N2 and then cooled to room temperature. The reaction mixture was poured into 100 mL ice/water. The aqueous layer was separated and saved. The CHCl3, layer was extracted three times with H2O (3×60 mL) and then discarded. The combined aqueous solution was neutralized with NaHCO3 powder to about pH 7-8. The resulting white precipitate was collected by suction filtration, washed with H2O (30 mL) and then dried under vacuum at 50° C. for 24 h. Yield: 85%.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US08828204B2 |
| 출처 데이터셋 | uspto-grants-2014_09 |
| ORD ID | ord-3627ce1f1bd04a75bfb9c11281d2ea87 |
| 출처 메모 | uspto-grants-2014_09 |