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Sulfuric acid magnesium salt (1:1) → Tert-butyl 2-(1-methylpiperidin-4-yl)hydrazinecarboxylate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Sulfuric acid magnesium salt (1:1) | HCID 24083 | — |
| 反応物 | tert-Butyl carbazate | HCID 70091 | — |
| 反応物 | 1-Methyl-4-piperidone | HCID 74049 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | Tert-butyl 2-(1-methylpiperidin-4-yl)hydrazinecarboxylate | HCID 68313226 | 63.4% |
反応手順
To a solution of 1-methylpiperidin-4-one (3.0 g, 27 mmol) in DCM (60 mL) was added MgSO4 (6.5 g, 54 mmol) and tert-butyl hydrazinecarboxylate (2.9 g, 22 mmol). The reaction mixture was heated to reflux overnight. The solid was filtered off and the filtrate was concentrated. The residue was purified by silica gel chromatography eluting with EtOAc/petroleum ether (1:20) to give tert-butyl 2-(1-methylpiperidin-4-yl)hydrazinecarboxylate (3.2 g, 53% yield) as a colorless oil. LCMS (ESI) m/z: 228.3 [M+H+].
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US09090628B2 |
| 出典データセット | uspto-grants-2015_07 |
| ORD ID | ord-043f25c0f9a941c89c9ad3c17e94a60a |
| 出典メモ | uspto-grants-2015_07 |