참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Phosphoric Acid | HCID 1004 | — |
| 반응물 | Sodium Hydroxide | HCID 14798 | — |
| 반응물 | Phosphorus oxide (P4O10) | HCID 14812 | — |
| 반응물 | 2,4-Hexanedione | HCID 76355 | — |
| 반응물 | 6-amino-4-(3-bromophenyl)-1-ethyl-2(1H)-pyridone | HCID 18969174 | — |
| 생성물 | 4-(3-bromophenyl)-1,7-diethyl-5-methyl-1,8-naphthyridin-2(1H)-one | HCID 9929331 | 73% |
반응 단계
A mixture of diphosphorus pentoxide (10.4 g) and phosphoric acid (5 ml) was stirred at 140° C. until it became transparent. Then, 6-amino-4-(3-bromophenyl)-1-ethyl-2(1H) -pyridone (2.5 g, 8.5 mmol) and 2,4-hexanedione (1.1 ml) were added to this solution, and the mixture was stirred at 140° C. for 3 hours. The reaction solution was poured into ice water, made alkaline by adding 1N sodium hydroxide aqueous solution and then extracted with ethyl acetate. After drying the organic layer with anhydrous magnesium sulfate, magnesium sulfate was removed by filtration and the filtrate was concentrated under reduced pressure. The resulting residue was then purified by silica gel column chromatography (benzene-ethyl acetate) to give 4-(3-bromophenyl)-1,7-diethyl-5-methyl-1,8-naphthyridin-2(1H)-one (2.3 g, 73%).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US05817670 |
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| 출처 데이터셋 | uspto-grants-1998_10 |
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| ORD ID | ord-093ccdb530794f02ac1f966978b12bc8 |
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| 출처 메모 | uspto-grants-1998_10 |
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