참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Ammonia | HCID 222 | — |
| 반응물 | Dacthal | HCID 2943 | — |
| 반응물 | 7-Aminocephalosporanic acid | HCID 441328 | — |
| 반응물 | HCID 178482017 | HCID 178482017 | — |
| 용매 | Acetonitrile | HCID 6342 | — |
| 생성물 | 7-Amino-3-(1-methyltetrazol-5-ylthiomethyl)-3-cephem-4-carboxylicacid | HCID 13020813 | 94.7% |
반응 단계
A 320 ml portion of acetonitrile was added to 54.5 g of 7-ACA and 25,6 g of 5-mercapto-1-methyl-1H-tetrazole, and 296.7 g of DCPA was added to the mixture with stirring and under cooling at -20° to -10° C. After the dissolution, the reaction mixture was stirred at 15° to 17° C. for 40 minutes to allow the reaction to proceed, cooled and poured into 1.8 kg of ice-water. The mixture was allowed to stand at 5° C. overnight, cooled by adding ice under stirring and adjusted to pH 4.0 with 25% aqueous ammonia. The resulting precipitate was recovered by filtration, washed with 480 ml of cold water and 500 ml of acetone successively, and dried, thereby affording 62.2 g (94.7% of yield) of 7-amino-3-(1-methyl-1H-tetrazol-5-yl)thiomethyl-3-cephem-4-carboxylic acid.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US04446318 |
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| 출처 데이터셋 | uspto-grants-1984_05 |
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| ORD ID | ord-74d13e00dc9a4f928fcd1a78a53aa853 |
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| 출처 메모 | uspto-grants-1984_05 |
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