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Bromide ion → 1-Boc-4-Methylenepiperidine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Bromide ion | HCID 259 | — |
| 反応物 | tert-Butyl 4-oxopiperidine-1-carboxylate | HCID 735900 | — |
| 反応物 | HCID 178418922 | HCID 178418922 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | 1-Boc-4-Methylenepiperidine | HCID 2756808 | 95.9% |
反応手順
47.2 g of methyltoluphenylphosphonium bromide and 21.9 g of tert-butyl 4-oxo-1-piperidinecarboxylate were added to a mixture of 14.8 g tert-butoxy potassium and 300 ml tetrahydrofuran, and stirred for 40 min at room temperature. The reaction solution was evaporated, diethyl ether was added thereto, and then filtered through Celite. The filtrate was washed with water and brine, dried over anhydrous magnesium sulfate, and then filtered. The filtrate was evaporated, and the resulting residue was subjected to silica gel column chromatography to give 20.8 g of tert-butyl 4-methylene-1-piperidinecarboxylate.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06699870B2 |
| 出典データセット | uspto-grants-2004_03 |
| ORD ID | ord-aea03e6a9ab1404ab6329c48f4861d88 |
| 出典メモ | uspto-grants-2004_03 |