関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Diisopropylethylamine | HCID 81531 | — |
| 反応物 | Methanaminium, N-((1H-benzotriazol-1-yloxy)(dimethylamino)methylene)-N-methyl-, hexafluorophosphate(1-) (1:1) | HCID 2733084 | — |
| 反応物 | 1-(Cyclohexylcarbonyl)piperazine | HCID 3437502 | — |
| 反応物 | Ethylacetate methanol | HCID 21584119 | — |
| 反応物 | HCID 59767741 | HCID 59767741 | — |
| 生成物 | HCID 131726981 | HCID 131726981 | — |
反応手順
To a stirred solution of 2-(4-oxo-3,4-dihydro-phthalazin-1-ylmethyl)-isonicotinic acid (iva) (0.25 g, 0.89 mol) in diemthylacetamide (2 mL) was added cyclohexyl-piperazin-1-yl-methanone (0.20 g, 1.0 mmol) followed by HBTU (0.38 g, 1.0 mmol) and diisopropyl ethyl amine (0.35 mL, 20.0 mmol) and stirred. The reaction mixture was then concentrated in vacuo and resulting oil subjected to flash chromatography eluent 9:1 EtOAc/MeOH. (rf of 0.3) The titled compound was isolated as a white solid. Single peak in LC-MS analysis, (0.18 g, 56%); m/z (LC-MS, ESP), RT=4.07 mins, (M+H)=460; 1H NMR (300 MHz) 12.57 (1H, S-NH), 8.56 (1H, d, J 5.1 Hz), 8.26 (1H, dd, J 1.5, 8.1 Hz), 7.95-7.80 (3H, m), 7.38 (1H, S), 7.25 (1H, d, J 5.7 Hz), 4.51 (2H, S), 3.56-3.17 (8H, m), 2.58 (1H, m), 1.71-1.61 (5H, m), 1.38-1.22 (5H, m).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US07407957B2 |
|---|
| 出典データセット | uspto-grants-2008_08 |
|---|
| ORD ID | ord-4ff2aa88688a40b190589f80c97e9b7e |
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| 出典メモ | uspto-grants-2008_08 |
|---|
