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Ammonium formate → Tetraethyl 3-aminooctane-1,1-bisphosphonate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Ammonium formate | HCID 2723923 | — |
| 反応物 | Tetraethyl 3-nitrooctane-1,1-bisphosphonate | HCID 19689057 | — |
| 触媒 | Palladium | HCID 23938 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 生成物 | Tetraethyl 3-aminooctane-1,1-bisphosphonate | HCID 19689051 | 95% |
反応手順
To a stirred solution of tetraethyl 3-nitrooctane-1,1-bisphosphonate (0.70 g, 1.62 mmol) in methanol (4 mL) was added ammonium formate (0.45 g, 6.9 mmol) and 10% palladium on carbon (0.070 g). After 24 hours, more 10% palladium on carbon (0.035 g) and ammonium formate (0.45 g, 6.9 mmol) were added. After stirring for a total of 4 days, the reaction mixture was filtered, rinsing the residue with methanol, and concentrated. The residue was taken up in brine (5 mL) and extracted with dichloromethane (4×15 mL), dried (Na2SO4) and concentrated to give the title compound (0.60 g, 95%) as an oil.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05728650 |
| 出典データセット | uspto-grants-1998_03 |
| ORD ID | ord-6f9159e7c4774638b827a4db2641898a |
| 出典メモ | uspto-grants-1998_03 |