참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | 4-Hydroxypyrrolidine | HCID 98210 | — |
| 반응물 | 1,1'-(9,9-Dimethyl-9H-xanthene-4,5-diyl)bis(1,1-diphenylphosphine) | HCID 636044 | — |
| 반응물 | Sodium t-butoxide | HCID 23676156 | — |
| 반응물 | 3-Bromo-6-chloro-2-methoxypyridine | HCID 53217454 | — |
| 촉매 | Bis(dibenzylideneacetone)palladium | HCID 9811564 | — |
| 용매 | Toluene | HCID 1140 | — |
| 생성물 | 1-(6-Chloro-2-methoxypyridin-3-yl)pyrrolidin-3-ol | HCID 86698850 | 5.9% |
반응 단계
A vial was charged 3-bromo-6-chloro-2-methoxypyridine(0.50 g, 2.2 mmol), pyrrolidin-3-ol (0.39 g, 4.5 mmol), tris(dibenzylideneacetone)dipalladium(0) (0.10 g, 0.10 mmol), Xantphos (0.13 g, 0.20 mmol), sodium tertbutoxide (0.32 g, 3.4 mmol) and toluene (5 mL). The mixture was purged with nitrogen then sealed. The mixture was heated to 100° C. overnight. The mixture was cooled to room temperature, filtered and diluted with 15 mL of water. The solution was extracted with ethyl acetate (10 mL×3). The organic layers were combined, dried over sodium sulfate, filtered and concentrated. The resulting residue was purified by silica gel chromatography to give the title compound (29.5 mg, 5.7%) as light brown solid.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US08889730B2 |
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| 출처 데이터셋 | uspto-grants-2014_11 |
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| ORD ID | ord-2014129b9bf646299b3f03df976cf9a2 |
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| 출처 메모 | uspto-grants-2014_11 |
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