참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Water | HCID 962 | — |
| 반응물 | 2-Fluorobenzoyl chloride | HCID 9808 | — |
| 반응물 | 2-(1H-Pyrrol-1-yl)isoindoline-1,3-dione | HCID 853719 | — |
| 용매 | 1,1-Dichloroethane | HCID 6365 | — |
| 생성물 | HCID 13457715 | HCID 13457715 | 19.1% |
반응 단계
To a mixture of N-phthalimidopyrrole (10 g, 47 mmole) and fused zinc chloride (10 g, 73 mmole) in 80 ml dichloroethane was added o-fluorobenzoyl chloride (7.5 g, 47 mmole). The reaction mixture was stirred at ambient temperature for twenty hours and at 80° for one hour. Thereafter, it was cooled, poured into water and extracted with dichloromethane. The organic extract was washed with water and with saturated sodium chloride solution, and dried over magnesium sulfate. The solution was filtered and evaporated to an oil which yielded a solid upon trituration with ethanol (yield 11 g, m.p. 180°-190°). This material was purified by column chromatography (silica gel, dichloromethane) to give 3 g solid. This material was recrystallized from isopropanol to give 2.6 g (17%) crystals, m.p. 202°-203°.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US04588727 |
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| 출처 데이터셋 | uspto-grants-1986_05 |
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| ORD ID | ord-f2380600dd884d9aaa5ae237f813d429 |
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| 출처 메모 | uspto-grants-1986_05 |
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