참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Hydrochloric Acid | HCID 313 | — |
| 반응물 | Ethyl Acetate | HCID 8857 | — |
| 반응물 | Thionyl Chloride | HCID 24386 | — |
| 반응물 | 2-Propenoic acid, 3-(4-nitrophenyl)- | HCID 70156 | — |
| 용매 | Dimethylformamide | HCID 6228 | — |
| 생성물 | 3-(4-nitrophenyl)prop-2-enoyl Chloride | HCID 319463 | 99.2% |
반응 단계
193.2 g (1 mole) of 4-nitrocinnamic acid and 650 g of ethyl acetate were placed in a reaction vessel. While 200 g of thionyl chloride with some drops of DMF was dropped into the reaction mixture, the reaction mixture was refluxed with stirring until the generation of hydrogen chloride gas stopped. The reacted solution was concentrated until a solid could be precipitated and then poured into hexane. The precipitated solid was separated by filtration and dried. 210 g of 4-nitrocinnamoyl chloride was yielded. 63.5 g (0.3 mole) of 4nitrocinnamoyl chloride and 400 g of methylethylketone were placed in a reaction vessel and the reaction mixtures were stirred by heating at 50° C. under a nitrogen current. 15.42 g (0.14 mole) of resorcinol, 32 g of pyridine, and 100 g of methylethylketone were added dropwise to the above reaction vessel using a dropping funnel. After the completion of the addition, the reaction solution was refluxed with stirring under a nitrogen current for 2 hours. After the reaction, the precipitate was separated by filtration and the filtrated solid was washed by water and dried. 64 g of white colored crystals (1,3-bis(4-nitrocinnamic acid) benzene) was yielded.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US06303742B1 |
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| 출처 데이터셋 | uspto-grants-2001_10 |
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| ORD ID | ord-5003da8c5d184c6ab6a738b1a8524c3d |
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| 출처 메모 | uspto-grants-2001_10 |
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