참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Piperidin-4-ol | HCID 79341 | — |
| 반응물 | Diisopropylethylamine | HCID 81531 | — |
| 반응물 | 3-Chloro-5-fluoro-4-iodopyridine | HCID 11032545 | — |
| 용매 | Ethyl Acetate | HCID 8857 | — |
| 용매 | N-methyl-2-pyrrolidone | HCID 13387 | — |
| 생성물 | 1-(3-Chloro-5-fluoro-4-pyridyl)piperidin-4-ol | HCID 86720960 | — |
반응 단계
To a solution of 3-chloro-5-fluoro-4-iodo-pyridine (1 g, 3.885 mmol) in NMP (1 mL) was added DIPEA (753.1 mg, 1.015 mL, 5.828 mmol) and piperidin-4-ol (589.4 mg, 5.828 mmol) and the mixture heated to 120° C. for 4 hours. The mixture was diluted with ethyl acetate (30 ml), washed twice with water (20 ml) and with brine. The organic layer was dried with MgSO4 and concentrated in vacuo to a yellow solid that was purified by column chromatography using DCM and then 2% MeOH/DCM as eluent, yielding 1-(3-chloro-5-fluoro-4-pyridyl)piperidin-4-ol. MS (ES+) 231.0.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 특허 번호 | US09340546B2 |
|---|
| 출처 데이터셋 | uspto-grants-2016_05 |
|---|
| ORD ID | ord-ca8aac4f5de04a68bae78c35d1f8096e |
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| 출처 메모 | uspto-grants-2016_05 |
|---|
