Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Potassium Phosphate, Tribasic → 6,7-dichloro-2-(4-(trifluoromethyl)pyridin-3-yl)-3,4-dihydroisoquinolin-1(2H)-one
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Potassium Phosphate, Tribasic | HCID 62657 | — |
| 반응물 | 6,7-Dichloro-3,4-dihydro-2H-isoquinolin-1-one | HCID 14177101 | — |
| 반응물 | 3-Bromo-4-(trifluoromethyl)pyridine | HCID 19937263 | — |
| 촉매 | Copper iodide | HCID 83717 | — |
| 용매 | 1,4-Dioxane | HCID 31275 | — |
| 생성물 | 6,7-dichloro-2-(4-(trifluoromethyl)pyridin-3-yl)-3,4-dihydroisoquinolin-1(2H)-one | HCID 56943054 | 8.4% |
반응 단계
Using an analogous procedure and workup as described for the preparation of Example 1A above, 6,7-dichloro-3,4-dihydroisoquinolin-1(2H)-one (I-55d: 100 mg, 0.463 mmol) was reacted with 3-bromo-4-(trifluoromethyl)pyridine (115 mg, 0.509 mmol), 1,4-dioxane (3 mL), copper iodide (7 mg, 0.046 mmol), trans-N,N′-dimethyl-cyclohexyl-1,2-diamine (20 mg, 0.1388 mmol) and potassium phosphate (245 mg, 1.157 mmol) in a sealed tube at 120° C. for 16 hours to afford the crude product. Purification by column chromatography on silica gel (20% ethylacetate in hexane) afforded 14 mg of the product (8.3% yield).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US08946260B2 |
| 출처 데이터셋 | uspto-grants-2015_02 |
| ORD ID | ord-0b202715be644a648d4a135f342adfd8 |
| 출처 메모 | uspto-grants-2015_02 |