関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | Sodium Dithionite | HCID 24489 | — |
| 反応物 | 3-(Difluoromethoxy)benzaldehyde | HCID 2736985 | — |
| 反応物 | (R)-1-(6-amino-5-nitropyridin-2-yl)-N,N-dimethylpiperidine-3-carboxamide | HCID 117966493 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | HCID 178484578 | HCID 178484578 | — |
反応手順
Into a 4 mL vial was added (R)-1-(6-amino-5-nitropyridin-2-yl)-N,N-dimethylpiperidine-3-carboxamide (500 μL, 0.3M) dissolved in N,N-dimethylformamide followed by 3-(difluoromethoxy)benzaldehyde (950 μL, 0.158M) dissolved in N,N-dimethylformamide. Water (50 μL) was added followed by sodium hydrosulfite (574 μmol) under a nitrogen atmosphere. The vial was capped and shaken at 110° C. for 18 h. The solvent was removed by Speedvac and the residue was purified by HPLC to afford the title compound. MS (API-ES+) (M+H) 416.2; HPLC retention time 1.392 min (Method E).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US09296745B2 |
|---|
| 出典データセット | uspto-grants-2016_03 |
|---|
| ORD ID | ord-c5c7fde5f03248d9b72f1696363a3fad |
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| 出典メモ | uspto-grants-2016_03 |
|---|
