참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Water | HCID 962 | — |
| 반응물 | 4-Nitro-m-toluidine | HCID 11898 | — |
| 반응물 | Methacryloyl chloride | HCID 13528 | — |
| 용매 | Dimethylacetamide | HCID 31374 | — |
| 생성물 | 2-Methyl-N-(3-methyl-4-nitrophenyl)acrylamide | HCID 45097643 | — |
반응 단계
3-Methyl-4-nitroaniline (2.0 g, 13 mmol) in N,N-dimethylacetamide (DMAC) (6 ml) was added dropwise to a cooled solution of methacryloyl chloride (2.0 ml, 20.7 mmol) in a nitrogen atmosphere while the temperature of the reaction mixture was maintained between 0-5° C. The solution was allowed to warm to room temperature and the mixture was stirred over night. The mixture was poured into water (70 ml) and extracted with ethyl acetate (4×40 ml). The organic phase was washed with saturated Na2CO3 (3×20 ml) and water (1×50 ml), dried over Na2SO4 and evaporated. The yield of the crude product was 4.17 g (contains DMA, theoretical yield 2.9 g), and it was used without further purifications. 1H NMR (DMSO-d6): 1.97 (3H, s), 2.55 (3H, s), 5.62 (1H, m), 5.96 (1H, m), 7.80 (2H, m), 8.05 (1H, m), 10.22 (1H, s).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US07390923B2 |
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| 출처 데이터셋 | uspto-grants-2008_06 |
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| ORD ID | ord-14257930e63c499bab077596c16d2683 |
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| 출처 메모 | uspto-grants-2008_06 |
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