関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Dimethylformamide | HCID 6228 | — |
| 反応物 | O-Phenylenediamine | HCID 7243 | — |
| 反応物 | Triethylamine | HCID 8471 | — |
| 生成物 | 2(1H)-Quinoxalinone, 3,4-dihydro- | HCID 185949 | — |
反応手順
To a solution of o-phenylenediamine (4 g, 37.03 mmol) in DMF (30 mL) was added triethylamine (10.3 mL, 74.06) followed by ethyl-2-bromo acetate (4.53 mL, 40.73 mmol). The reaction was stirred at RT for 16 h and at 80° C. for 3 h. The reaction was monitored by TLC. After completion of reaction, the DMF was removed under vacuum. Water (20 mL) was added to the reaction mixture, which was then extracted with EtOAc (300 mL). The organic layer was dried over sodium sulfate, concentrated under vacuum, and the product recrystallized with DCM/hexane in 1:1 ratio to obtain 2.2 g of desired compound.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US09193728B2 |
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| 出典データセット | uspto-grants-2015_11 |
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| ORD ID | ord-6021c58e75c1457b949ae4f6c2098976 |
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| 出典メモ | uspto-grants-2015_11 |
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