참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Sodium hydride | HCID 24758 | — |
| 반응물 | Ammonium Chloride | HCID 25517 | — |
| 반응물 | Methyl 4-chlorophenylacetate | HCID 104196 | — |
| 반응물 | 1,2-Dichloro-4-fluoro-5-nitrobenzene | HCID 533951 | — |
| 용매 | Dimethylformamide | HCID 6228 | — |
| 생성물 | Methyl (4-chlorophenyl)(4,5-dichloro-2-nitrophenyl)acetate | HCID 86644371 | 336.3% |
반응 단계
A solution of 5 g of 1,2-dichloro-4-fluoro-5-nitrobenzene and 4.4 g of methyl 4-chlorophenylacetate in 70 ml of DMF is added, under a stream of nitrogen, to a suspension at −10° C. of 2.85 g of 60% NaH in 45 ml of DMF, and the temperature is maintained at −5° C. The mixture is reacted for 2 hours, while allowing the temperature to return to room temperature. The resulting mixture is poured onto ice, aqueous 10% NH4Cl solution is added and the mixture is extracted with ethyl acetate. The organic phase is dried, filtered and concentrated. 30 g of a brown oil are obtained, and are purified on a column with hexane and then with a 95/5 hexane/EtOAc mixture to give 3.18 g of oil.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US08202871B2 |
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| 출처 데이터셋 | uspto-grants-2012_06 |
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| ORD ID | ord-d3e024f642e44fe9ba56d7c4d6cdcc3b |
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| 출처 메모 | uspto-grants-2012_06 |
|---|