참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Water | HCID 962 | — |
| 반응물 | Trifluoroacetic acid | HCID 6422 | — |
| 반응물 | Butanedioic acid, 2-methyl-3-oxo-, 1,4-diethyl ester | HCID 97750 | — |
| 반응물 | (2,4-Dichlorophenyl)hydrazine monohydrochloride | HCID 2723905 | — |
| 용매 | Toluene | HCID 1140 | — |
| 생성물 | HCID 86760639 | HCID 86760639 | — |
반응 단계
2,4-dichlorophenylhydrazine hydrochloride(12.6 g) is dissolved in 100 ml of toluene and this solution is placed under nitrogen; after stirring, 10 g of diethyl 2-methyl-3-oxosuccinate are added and the mixture is then heated and 5 ml of TFA are added at 55° C. The mixture is left at the reflux of the solvent for 4 and a half hours, with stirring. The mixture is allowed to return to ambient temperature and is then heated to 75° C. and the reaction medium is hydrolyzed with 30 ml of water. The mixture is separated by settling out, the aqueous phase is discarded and the organic phase is then evaporated in order to eliminate the residual TFA. The organic phase is taken up with 10 ml of toluene and the expected product then crystallizes, m=10.2 g.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US07358371B2 |
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| 출처 데이터셋 | uspto-grants-2008_04 |
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| ORD ID | ord-abe29720067d431584a668e3a7708b84 |
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| 출처 메모 | uspto-grants-2008_04 |
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