Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
3,5-Dibromopyridine → 3-Bromo-5-(prop-1-en-2-yl)pyridine
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | 3,5-Dibromopyridine | HCID 69369 | — |
| 반응물 | Sodium Carbonate Decahydrate | HCID 151402 | — |
| 반응물 | 4,4,5,5-Tetramethyl-2-(prop-1-en-2-yl)-1,3,2-dioxaborolane | HCID 10997426 | — |
| 반응물 | Potassium acetate hydrate | HCID 23702041 | — |
| 촉매 | HCID 178418807 | HCID 178418807 | — |
| 용매 | Acetonitrile | HCID 6342 | — |
| 생성물 | 3-Bromo-5-(prop-1-en-2-yl)pyridine | HCID 23436808 | 52% |
반응 단계
A mixture of [1,1′-bis(diphenylphosphino)ferrocene]dichloropalladium(II) dichloromethane adduct; 98.0 mass %, potassium acetate hydrate (7.4997 mmol; 3.7 mL), sodium carbonate decahydrate (7.4997 mmol; 3.7 mL), Acetonitrile (15 mL) and 3,5-dibromopyridine (4.9998 mmol; 1184.4 mg) in 2-isopropenyl-4,4,5,5-tetramethyl-1,3,2-dioxaborolane (4.9998 mmol; 840.0 mg; 0.940 mL) in a pressure tube was heated under microwave at 120° C. for 3 min. The mixture was cooled to room temperature. The layers were separated. The aqueous layer was extracted with EtOAc. The combined organic layer was concentrated. The residue was purified on silica eluted with 0 to 10% MeOH in DCM to afford 3-bromo-5-isopropenyl-pyridine as a dark tan solid (512.6 mg, 52%).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US09434725B2 |
| 출처 데이터셋 | uspto-grants-2016_09 |
| ORD ID | ord-09526792083b4bb8a99e50999cd69c27 |
| 출처 메모 | uspto-grants-2016_09 |