참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Water | HCID 962 | — |
| 반응물 | Dimethylformamide dimethyl acetal | HCID 78373 | — |
| 반응물 | Acetanilide, 3'-acetyl-2,2,2-trifluoro- | HCID 673706 | — |
| 용매 | Dimethylformamide | HCID 6228 | — |
| 생성물 | N-[3-(3-dimethylamino-1-oxo-2-propenyl)phenyl]-methylamine | HCID 67198189 | 55% |
반응 단계
8.37 g (36.21 mmol) de N-(3-acetylphenyl)-2,2,2-trifluoro-acetamide were dissolved in 80 ml of N,N-dimethyl formamide. To the resultant solution 24.23 ml (181.02 mmol) of N,N-dimethylformamide dimethyl acetal were added and heated at 150° C. for 2 h. The solvent was removed by reduced pressure distillation to yield an oil which was treated with 50 ml of water and extract with 3×100 ml of dichloromethane. The organic layers were washed with 2×200 ml of a saturated solution of sodium chloride, dried over anhydrous sodium sulfate and evaporated to dryness by reduced pressure distillation. A solid was obtained, which precipitated from a mixture of ethanol-ethyl ether to give 4.1 g (yield=55%) of 3-(dimethylamino)-1-[3-(methylamino)phenyl]prop-2-en-1-one.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US07947688B2 |
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| 출처 데이터셋 | uspto-grants-2011_05 |
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| ORD ID | ord-449cbc86ef6049d8bef39eba40a3139a |
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| 출처 메모 | uspto-grants-2011_05 |
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