関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | 2-Bromo-6-fluoropyridine | HCID 639438 | — |
| 反応物 | tert-butyl N-(6-methylpiperidin-3-yl)carbamate | HCID 42609251 | — |
| 溶媒 | Dimethyl Sulfoxide | HCID 679 | — |
| 生成物 | tert-butyl N-[1-(6-bromo-2-pyridyl)-6-methyl-3-piperidyl]carbamate | HCID 86707072 | 39% |
反応手順
A solution containing 2-bromo-6-fluoropyridine (0.95 mL, 6.65 mmol and tert-butyl 6-methylpiperidin-3-ylcarbamate (750 mg, 3.32 mmol) in methyl sulfoxide 5.0 ml was heated 95° C. 18 h. The reaction was quenched with water then extracted with EtOAc. The organic layers was dried with sodium sulfate, filtered, and concentrated in vacuum. The crude product was purified by flash chromatography (EtOAc/Heptane eluted at 30% EtOAc) to give tert-butyl N-[1-(6-bromo-2-pyridyl)-6-methyl-3-piperidyl]carbamate (480 mg) in 39% yield. MS (ESI) m/z: 371.2
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US09434725B2 |
|---|
| 出典データセット | uspto-grants-2016_09 |
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| ORD ID | ord-3d401b61bbcc445dbb22ecc949716f4e |
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| 出典メモ | uspto-grants-2016_09 |
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