참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Cesium carbonate | HCID 10796 | — |
| 반응물 | Binap, (A+-)- | HCID 634876 | — |
| 반응물 | Tert-butyl Piperazine-1-carboxylate Hydrochloride | HCID 2755973 | — |
| 반응물 | 5-Bromo-2-fluoropyridine | HCID 2783168 | — |
| 촉매 | palladium(II) acetate | HCID 167845 | — |
| 용매 | Water | HCID 962 | — |
| 용매 | Toluene | HCID 1140 | — |
| 용매 | Hexane | HCID 8058 | — |
| 용매 | Ethyl Acetate | HCID 8857 | — |
| 생성물 | Tert-butyl 4-(6-fluoropyridin-3-yl)piperazine-1-carboxylate | HCID 59834735 | 43% |
반응 단계
A suspension of piperazine-1-carboxylic acid tert-butyl ester hydrochloride (0.75 mmol), 5-bromo-2-fluoropyridine (0.90 mmol), (R)-2,2′-bis(diphenylphosphino)-1, 1′-binaphthyl (0.038 mmol), palladium acetate (0.038 mmol) and cesium carbonate (1.8 mmol) in toluene is stirred at 80° C. for 7 h and then 100° C. for 4 h, and poured into water. The mixture is extracted with AcOEt. The organic layer is washed with water, dried over magnesium sulfate, and concentrated. The crude product is purified by silica gel column chromatography to give the product in 43% yield. Rf=0.61 (n-hexane:AcOEt=1:1)
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 특허 번호 | US07452886B2 |
|---|
| 출처 데이터셋 | uspto-grants-2008_11 |
|---|
| ORD ID | ord-61ffb66676194eb78c51d58eeeef3fb6 |
|---|
| 출처 메모 | uspto-grants-2008_11 |
|---|
