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Triethylamine → (S)-N-[1-(amino-imino-methyl)-piperidin-3-ylmethyl]-benzamide (R)-hydroxy-phenylacetate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | Methanesulfonic acid, aminoimino- | HCID 9877361 | — |
| 反応物 | (R)-N-piperidin-3-ylmethyl-benzamide (R)-hydroxy-phenyl-acetate | HCID 70050196 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | (S)-N-[1-(amino-imino-methyl)-piperidin-3-ylmethyl]-benzamide (R)-hydroxy-phenylacetate | HCID 86748615 | 62.4% |
反応手順
Bc) 19.3 g of the mandelic acid salt obtained under Bb) are suspended in 193 ml of DMF, treated with 21.7 ml of triethylamine and 7.75 g of formamidinesulfonic acid and stirred at room temperature. The reaction mixture is evaporated and the residue is chromatographed on RP-18 silica gel with a water-acetonitrile gradient. There are isolated 13.4 g of (S)-N-[1-(amino-imino-methyl)-piperidin-3-ylmethyl]-benzamide (R)-hydroxy-phenyl-acetate (1:1), MS (FAB): 218 M-(H2N--CN).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05677448 |
| 出典データセット | uspto-grants-1997_10 |
| ORD ID | ord-2c73f8d2c19a425893bff09943551c0a |
| 出典メモ | uspto-grants-1997_10 |