참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | 4,4'-Difluorobenzophenone | HCID 9582 | — |
| 반응물 | Potassium Carbonate | HCID 11430 | — |
| 반응물 | 2-Allylphenol | HCID 15624 | — |
| 반응물 | 4-Fluorobenzophenone | HCID 67663 | — |
| 용매 | Toluene | HCID 1140 | — |
| 용매 | N-methyl-2-pyrrolidone | HCID 13387 | — |
| 생성물 | HCID 86742606 | HCID 86742606 | — |
반응 단계
o-Allylphenol (52.2 g), 4,4'-difluorobenzophenone (35 g), 4-fluorobenzophenone (13.8 g), potassium carbonate (37.75 g), dry N-methylpyrrolidone (200 ml) and toluene (75 ml) are placed in a 3-necked 1500 ml flask fitted with a stirrer, reflex condensor and thermometer and the mixture is heated under nitrogen to a temperature between 155°-160° C. and stirred for 3 hours. Water and toluene are separated via a Dean Stark trap and finally after 3 hours the reaction mixture reaches a temperature of 160° C. The mixture is cooled to 100° C. and a 1:1 mixture of toluene/water (400 ml) is added while stirring. After phase separation the aqueous layer is washed with toluene (100 ml) and the combined toluene layers are washed 4 times with water (150 ml). The toluene phase is dried over sodium sulphate and toluene distilled off by use of a rotary evaporator finally in vacuum leaving a 4,4'-bis[o-(1-propenyl)phenoxy]benzophenone/4-[o-(1-propenyl)phenoxy]benzophenone mixture as a light yellow melt. The yield is 89 g.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US04789704 |
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| 출처 데이터셋 | uspto-grants-1988_12 |
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| ORD ID | ord-eb6fcc868bd5423189fa7be8c72096f1 |
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| 출처 메모 | uspto-grants-1988_12 |
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