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4-Chloropyridine → tert-Butyl [1-(pyridin-4-yl)piperidin-4-yl]carbamate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 4-Chloropyridine | HCID 12288 | — |
| 反応物 | 4-(N-Boc-amino)piperidine | HCID 723833 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 溶媒 | n-butanol water NEt3 | HCID 86625244 | — |
| 生成物 | tert-Butyl [1-(pyridin-4-yl)piperidin-4-yl]carbamate | HCID 18008972 | — |
反応手順
A solution of 3 g Piperidin-4-yl-carbamic acid tert-butyl ester and 2.5 g 4-Chloropyridine in 9 ml n-butanol/water/NEt3 1:1:1 was heated at 100° C. for 48 h. Then the solution was cooled to RT diluted with DCM and washed with NaHCO3 solution and water. The organic layer was dried over Na2SO4, filtered, and the solvent was removed under reduced pressure. Chromatographic purification of the residue on silica with DCM as eluent gave after evaporation of the fractions containing the product a white foam. Yield 1.7 g.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07429581B2 |
| 出典データセット | uspto-grants-2008_09 |
| ORD ID | ord-67cb0225ae7f4dc89bfb109598d6f565 |
| 出典メモ | uspto-grants-2008_09 |