참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | 1-Chloro-2-nitrobenzene | HCID 6945 | — |
| 반응물 | 2,2,2-Trifluoro-N-(hydroxymethyl)acetamide | HCID 3084931 | — |
| 용매 | Sulfuric Acid | HCID 1118 | — |
| 생성물 | N-(4-chloro-3-nitrobenzyl)-2,2,2-trifluoroacetamide | HCID 19879857 | 30,891.9% |
반응 단계
To a solution of 1-chloro-2-nitrobenzene (10.0 g, 0.063 mmol) in conc. sulphuric acid (150 mL) was added N-hydroxy methyl trifluoro acetamide (9.98 g, 0.069 mmol). The reaction mixture was heated at 70-80° C. for 24 h. The reaction mass was quenched in ice cold water, neutralised with sodium hydroxide and extracted with DCM. The organic layer was concentrated and the obtained crude product was purified by column chromatography on silica gel eluting with 4% EtOAc: pet. ether to afford 5.5 g of desired product. 1H NMR (300 MHz, DMSO d6): 4.48 (d, J=3.9 Hz, 2H), 7.62-7.64 (m, 1H), 7.72-7.78 (m, 1H), 7.97-8.01 (m, 1H), 10.09 (brs, 1H).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US09439890B2 |
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| 출처 데이터셋 | uspto-grants-2016_09 |
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| ORD ID | ord-d0adaacf7d1f472794d4e88810d0c6df |
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| 출처 메모 | uspto-grants-2016_09 |
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