関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Isopropanol | HCID 3776 | — |
| 反応物 | Diaminomaleonitrile | HCID 2723951 | — |
| 反応物 | HCID 57831019 | HCID 57831019 | — |
| 生成物 | 6-ethyl-9-oxo-9H-indeno[1,2-b]pyrazine-2,3-dicarbonitrile | HCID 57831024 | — |
反応手順
A suspension of 29c (298 mg, 1.71 mmol) and diaminomaleonitrile (185 mg, 1.71 mmol) in iPrOH (17 ml) was stirred at 80° C. for 20 h. The solvent was evaporated under reduced pressure and the crude was purified by flash chromatography (CH2Cl2). The obtained product was purified by preparative HPLC, obtaining 32 as yellow solid as 7:3 regioisomeric mixture with the 7-ethyl analogue. 1H NMR (300 MHz, CDCl3): main product: δ 7.95 (d, 1H), 7.80 (m, 1H), 7.67 (bd, 1H), 2.83 (q, 2H), 1.33 (t, 3H); minority product: δ 7.89 (d, 1H), 7.89 (m, 1H), 7.56 (bd, 1H), 2.86 (q, 2H), 1.36 (t, 3H). ESI+MS: calcd for C15H8N4O: 260.26; found: 261.1 (MH+).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08648076B2 |
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| 出典データセット | uspto-grants-2014_02 |
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| ORD ID | ord-2ecba929284b42688b3bc34e18d072dc |
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| 出典メモ | uspto-grants-2014_02 |
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