참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | N,N-Dimethylaniline | HCID 949 | — |
| 반응물 | Triethylamine | HCID 8471 | — |
| 반응물 | 2,2,2-Trichloroethyl 2-methyl-7-amino-3-cephem-4-carboxylate hydrochloride | HCID 12834135 | — |
| 반응물 | Benzylthiocarbonyl chloride | HCID 19906501 | — |
| 용매 | Dichloromethane | HCID 6344 | — |
| 생성물 | HCID 131711252 | HCID 131711252 | 90.2% |
반응 단계
2,2,2-Trichloroethyl 2-methyl-7-amino-3-cephem-4-carboxylate hydrochloride (3.0 g) was suspended in dried dichloromethane (50 ml) and then dissolved by adding triethylamine (0.72 g) and dimethylaniline (1.9 g) under cooling at -15° C. To a mixture was dropwise added a solution of phenylthioacetyl chloride (2.2 g) in dried dichloromethane (10 ml) under stirring, and the mixture was stirred for 1.5 hours at the same temperature. After the reaction, the reaction mixture was in turn washed with 5% hydrochloric acid, water, 5% sodium bicarbonate aqueous solution and water and then dried. After the solvent was distilled off, ether was added to the residue, after which the precipitated crystals were collected by filtration and dried to give 2,2,2-trichloroethyl 2-methyl-7-(2-phenylthioacetamido)-3-cephem-4-carboxylate (3.4 g), mp 140° to 142° C.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US04385176 |
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| 출처 데이터셋 | uspto-grants-1983_05 |
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| ORD ID | ord-dcc77b214b0f4656adb3610d244174a5 |
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| 출처 메모 | uspto-grants-1983_05 |
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