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4-Methylmorpholine → (1-Methylpiperidin-4-yl)methyl 4-nitrophenyl carbonate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 4-Methylmorpholine | HCID 7972 | — |
| 反応物 | Bis(4-nitrophenyl) carbonate | HCID 78756 | — |
| 反応物 | 1-Methyl-4-piperidinemethanol | HCID 271971 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | (1-Methylpiperidin-4-yl)methyl 4-nitrophenyl carbonate | HCID 57445006 | 73.6% |
反応手順
(1-Methylpiperidin-4-yl)methanol (2.50 g, 19.3 mmol) in DCM (50 mL) was added to a solution of bis-(4-nitrophenyl)carbonate (7.06 g, 23.2 mmol) in DCM (100 mL), followed by NMM (1.70 mL, 15.5 mmol). The reaction mixture was stirred for 90 hours and then washed sequentially with aliquots of 1 M aq Na2CO3 solution until the aqueous layer was colourless. The organic layer was dried (MgSO4) and concentrated in vacuo to give (1-methylpiperidin-4-yl)methyl 4-nitrophenyl carbonate (4.18 g, 73%) as a yellow solid.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08093248B2 |
| 出典データセット | uspto-grants-2012_01 |
| ORD ID | ord-752a22679006497f8d1083d89e310ac5 |
| 出典メモ | uspto-grants-2012_01 |