참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Potassium Phosphate, Tribasic | HCID 62657 | — |
| 반응물 | 5-(Aminomethyl)-2-chloropyridine | HCID 7020927 | — |
| 반응물 | 2-Dicyclohexylphosphino-2',6'-dimethoxybiphenyl | HCID 11269872 | — |
| 반응물 | 2-(Trifluoromethyl)pyridine-4-boronic acid | HCID 45158880 | — |
| 촉매 | palladium(II) acetate | HCID 167845 | — |
| 용매 | (+-)-2-Butanol | HCID 6568 | — |
| 생성물 | HCID 67208623 | HCID 67208623 | — |
반응 단계
To a flask containing (6-chloropyridin-3-yl)methanamine 33-2 (375 mg, 2.63 mmol), 2-(trifluoromethyl)pyridin-4-ylboronic acid 33-1 (500 mg, 2.63 mmol), Pd(OAc)2 (34 mg, 0.15 mmol), 2-dicyclohexylphosphino-2′,6′-dimethoxybiphenyl (S-Phos) (124 mg, 0.30 mmol) and potassium phosphate (1.90 g, 9.00 mmol) under argon was added 2-butanol (4 mL). The mixture was stirred at 100° C. for 10 hours. After cooling to room temperature, the mixture was filtered through celite cake. The filtrate was diluted with ethyl acetate, washed with H2O and brine, dried over Na2SO4, and concentrated to dryness by rotary evaporation. The crude product was purified by silica gel flash chromatography, eluted with 5% methanol containing ˜7N ammonia in dichloromethane to give (2′-(trifluoromethyl)-2,4′-bipyridin-5-yl)methanamine 33-3 as a yellow solid. MS m/z 254.1 (M+1)
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US09181235B2 |
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| 출처 데이터셋 | uspto-grants-2015_11 |
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| ORD ID | ord-3bcf7431285b4be586bd389a0b629ac8 |
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| 출처 메모 | uspto-grants-2015_11 |
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