참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | 2,4-Dichloro-5-methoxyaniline | HCID 1476636 | — |
| 반응물 | Pyridinium chloride | HCID 10176127 | — |
| 반응물 | HCID 178486400 | HCID 178486400 | — |
| 용매 | Glycol monoethyl ether | HCID 8076 | — |
| 용매 | Sodium Bicarbonate | HCID 516892 | — |
| 생성물 | HCID 178486403 | HCID 178486403 | 65.6% |
반응 단계
A mixture of 0.7 g (2.46 mmol) of 4-chloro-8-hydroxy-7-methoxybenzo[g]quinoline-3-carbonitrile, 0.57 g (2.95 mmol) of 2,4-dichloro-5-methoxyaniline and 0.28 g (2.46 mmol) of pyridine hydrochloride in 7 mL of 2-ethoxyethanol is heated at 120° C. for 2 hours, then cooled to room temperature. The product mixture is diluted with saturated solution of sodium bicarbonate and stirred for 15 minutes. The resulting solid is collected by filtration, washed with water and dried. The crude product is purified by silica gel chromatography, utilizing a 98:2 to 90:10 gradient of methylene chloride/methanol to give 0.71 g of 4-(2,4-dichloro-5-methoxyphenylamino)-8-hydroxy-7-methoxybenzo[g]quinoline-3-carbonitrile as a yellow solid, mp, 238-240° C.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US06638929B2 |
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| 출처 데이터셋 | uspto-grants-2003_10 |
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| ORD ID | ord-e2d580160bfb4dcea4b7e35feca411e0 |
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| 출처 메모 | uspto-grants-2003_10 |
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