참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Methacrylic Acid | HCID 4093 | — |
| 반응물 | Disperse orange 3 | HCID 12896 | — |
| 반응물 | Sodium hydride | HCID 24758 | — |
| 용매 | Tetrahydrofuran | HCID 8028 | — |
| 생성물 | Disperse Orange 3 methacrylamide | HCID 4574980 | 56% |
반응 단계
0.6 g of sodium hydride was added carefully to a 3 neck flask equipped with a condenser, addition funnel, and magnetic bar. 75 ml of anhydrous THF was added and the mixture stirred for 10 minutes. A solution of 4.0 g 4-(4-nitrophenylazo)aniline in 75 ml THF was added drop-wise and the flask stirred at 50° C. The temperature was raised to 95° C., and the mixture was refluxed for 6 hrs. The mixture was allowed to cool to room temperature and then 6.0 g of methacrylic acid in 20 ml THF was added drop-wise. The mixture was again refluxed for 8 hrs. The solution was cooled to room temperature. THF was evaporated to reveal a dark orange solid. The solid was washed thoroughly with dilute HCl and water. The product was recrystallized in 95% methanol. The yield was 56%.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US07842367B2 |
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| 출처 데이터셋 | uspto-grants-2010_11 |
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| ORD ID | ord-9511b8526ed0454c9bd035cd15df1a1d |
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| 출처 메모 | uspto-grants-2010_11 |
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