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Sodium Iodide → Benzyl 4-((6-(tert-butoxycarbonylamino)pyridin-3-yl)methyl)piperazine-1-carboxylate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Sodium Iodide | HCID 5238 | — |
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | Benzyl piperazine-1-carboxylate | HCID 643495 | — |
| 反応物 | (6-(Tert-butoxycarbonylamino)pyridin-3-yl)methyl methanesulfonate | HCID 86641141 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | Benzyl 4-((6-(tert-butoxycarbonylamino)pyridin-3-yl)methyl)piperazine-1-carboxylate | HCID 67203742 | 96% |
反応手順
A mixture of (6-(tert-butoxycarbonylamino)pyridin-3-yl)methyl methanesulfonate (102; 1.30 g, 5.4 mmol), benzyl piperazine-1-carboxylate 103; (1.42 g, 6.5 mmol), K2CO3 (2.30 g, 16.1 mmol) and NaI (0.08 g, 0.54 mmol) in DMF (20 mL) was stirred at 60° C. for 2 h. The reaction mixture was filtered and the filtrate was concentrated under reduced pressure. Water (30 mL) was added and the mixture was filtered. The collected solids were washed further with water and dried to afford benzyl 4-((6-(tert-butoxycarbonylamino)pyridin-3-yl)methyl)piperazine-1-carboxylate 104 (2.20 g, 96%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08846947B2 |
| 出典データセット | uspto-grants-2014_09 |
| ORD ID | ord-d909f28cf0ec4418836cad7882ed2f2e |
| 出典メモ | uspto-grants-2014_09 |