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t-Butyl 3-(4-bromophenyl)-1-(methoxy(methyl)amino)-1-oxopropan-2-ylcarbamate → t-Butyl 1-(4-bromophenyl)-3-oxohexan-2-ylcarbamate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | t-Butyl 3-(4-bromophenyl)-1-(methoxy(methyl)amino)-1-oxopropan-2-ylcarbamate | HCID 18779134 | — |
| 反応物 | HCID 178455851 | HCID 178455851 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | t-Butyl 1-(4-bromophenyl)-3-oxohexan-2-ylcarbamate | HCID 66863791 | 56.9% |
反応手順
A solution of propylmagnesium bromide (29.7 g, 201.6 mmol, 3.0 equiv) in THF (200 mL) was added dropwise with stirring at 0° C. to a solution of the carbamate (26 g, 66.5 mmol, 1.0 equiv) in THF (200 mL). The resulting solution was stirred overnight at room temperature. The reaction was then quenched by the addition of aqueous NH4Cl (200 mL). The resulting solution was extracted with EtOAc and the organic layers combined. The resulting mixture was washed with saturated NaHCO3 (200 mL) and saturated aqueous NaCl (200 mL), then dried over anhydrous MgSO4. The residue was applied onto a silica gel column with petroleum ether/EtOAc (5:1) to yield t-butyl 1-(4-bromophenyl)-3-oxohexan-2-ylcarbamate (14 g) as a white solid.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US09181206B2 |
| 出典データセット | uspto-grants-2015_11 |
| ORD ID | ord-8a74778347054a6cb65034e4a68a45d3 |
| 出典メモ | uspto-grants-2015_11 |