関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | 2,6-Dichloropyridine | HCID 16989 | — |
| 反応物 | Sodium hydride | HCID 24758 | — |
| 反応物 | Tert-butyl 4-hydroxypiperidine-1-carboxylate | HCID 643502 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | Tert-butyl 4-[(6-chloropyridin-2-yl)oxy]piperidine-1-carboxylate | HCID 21906058 | 48% |
反応手順
To a stirred solution of 4-Hydroxy-piperidine-1-carboxylic acid tert-butyl ester (1.63 g, 8.1 mmol) in THF (20 mL), NaH (0.40 g, 10.1 mmol)) was added and stirred at 60° C. for 0.5 h. 2,6-dichloropyridine (1.0 g, 6.75 mmol) was added and stirred at room temperature for 3-4-h. The reaction was quenched with water and extracted with ethyl acetate. The organic layer was concentrated in vacuo and the resultant residue was purified by flash column chromatography to yield tert-butyl 4-((6-chloropyridin-2-yl)oxy)piperidine-1-carboxylate as a pale yellow solid (0.98 g, 48%); MS: 335.1 (M+23)
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US09000175B2 |
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| 出典データセット | uspto-grants-2015_04 |
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| ORD ID | ord-6b98d450d34d4947afe804c798f92a1c |
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| 出典メモ | uspto-grants-2015_04 |
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