참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Picolinic acid | HCID 1018 | — |
| 반응물 | Potassium Phosphate, Tribasic | HCID 62657 | — |
| 반응물 | Benzene, 1-bromo-4-(trifluoromethyl)- | HCID 67872 | — |
| 반응물 | 4-(2-Aminopyridin-3-yl)phenol | HCID 66748477 | — |
| 촉매 | Copper(1+) iodide; Copper(I) iodide; Cuprous iodide; Cuprous iodide (CuI) | HCID 24350 | — |
| 용매 | Dimethyl Sulfoxide | HCID 679 | — |
| 생성물 | 3-(4-(4-(Trifluoromethyl)phenoxy)phenyl)pyridin-2-amine | HCID 66747726 | 77.8% |
반응 단계
Copper(I) iodide (102 mg) was added to a mixture of picolinic acid (66.1 mg), 4-(2-aminopyridin-3-yl)phenol (500 mg), tripotassium phosphate (1710 mg), 1-bromo-4-(trifluoromethyl)benzene (725 mg) and DMSO (8 mL). The mixture was stirred at 130° C. under nitrogen for 5 hr. Activated carbon was added and the insoluble solid was removed by filtration through NH-silica gel/Celite pad (eluted with EtOAc). Water was added and the extracted organic layer was washed with brine. Silica-gel was added to the organic layer and the volatiles were removed in vacuo. The mixture supported on silica-gel was purified by column chromatography (NH-silica gel, eluted with EtOAc in hexane) to give the title compound (690.4 mg) as a yellow solid.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US08916551B2 |
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| 출처 데이터셋 | uspto-grants-2014_12 |
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| ORD ID | ord-d662b85572d644b3b3edd886a003e51e |
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| 출처 메모 | uspto-grants-2014_12 |
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