참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | 1,2-Dimethoxyethane | HCID 8071 | — |
| 반응물 | Sodium hydride | HCID 24758 | — |
| 반응물 | 4-[N,N-bis(3,4-dimethylphenyl)amino]benzaldehyde | HCID 22617091 | — |
| 촉매 | Ethanol | HCID 702 | — |
| 촉매 | Tetramethylphosphonium bromide | HCID 357594 | — |
| 생성물 | 4-[N,N-bis(3,4-dimethylphenyl)amino]styrene | HCID 10892783 | — |
반응 단계
12.1 g of sodium hydride and 580 mL of 1,2-dimethoxyethane were placed in a three-neck flask, and while stirring at room temperature, 108.5 g of tetramethyl phosphonium bromide was added. After adding one drop of anhydrous ethanol, the mixture was reacted for 4 hours at 70° C. 100 g of 4-[N,N-bis-(3,4-dimethylphenyl) amino] benzaldehyde was added to the reaction mixture, and the mixture was reacted for 5 hours at 70° C. The reaction solution was filtered, and an ether extract of the filtered cake and filtrate were washed in water. The ether solution was dehydrated with calcium chloride. The ether was removed and the reaction mixture was obtained. This was recrystallized twice with ethanol, and a needle-form of 4-[N,N-bis-(3,4-dimethylphenyl) amino] styrene was obtained. The amount obtained was 84.5 g (yield rate of 85.0%).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US05824443 |
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| 출처 데이터셋 | uspto-grants-1998_10 |
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| ORD ID | ord-6da04a8708bd4fbda1faf628a53670a4 |
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| 출처 메모 | uspto-grants-1998_10 |
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