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Methylamine → trans-6-(2,5-Difluorophenyl)-1-methyl-5-nitropiperidin-2-one
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Methylamine | HCID 6329 | — |
| 反応物 | Methyl 4-nitrobutyrate | HCID 25604 | — |
| 反応物 | 2,5-Difluorobenzaldehyde | HCID 137663 | — |
| 溶媒 | Ethanol | HCID 702 | — |
| 生成物 | trans-6-(2,5-Difluorophenyl)-1-methyl-5-nitropiperidin-2-one | HCID 67389784 | — |
反応手順
To a solution of 2,5-difluorobenzaldehyde (0.765 mL, 7.04 mmol) in ethanol (15 mL) were added methyl 4-nitrobutyrate (0.901 mL, 7.04 mmol) and methylamine (7.04 mL, 14.07 mmol). The mixture was heated at reflux temperature overnight. After evaporation, the residue was purified by column chromatography (silica gel Biotage 40M) eluting with ethyl acetate/hexane (gradient from 40% to 60%) to give the title compound as the racemic trans isomer. LC-MS: 271.05 (M+1).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08653059B2 |
| 出典データセット | uspto-grants-2014_02 |
| ORD ID | ord-1e31ca7127cd4dd08659570443fd9ba5 |
| 出典メモ | uspto-grants-2014_02 |