참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Water | HCID 962 | — |
| 반응물 | 7-Aminocephalosporanic acid | HCID 441328 | — |
| 반응물 | Diphosphoryl tetrachloride | HCID 4432411 | — |
| 반응물 | HCID 178521532 | HCID 178521532 | — |
| 용매 | Acetonitrile | HCID 6342 | — |
| 생성물 | HCID 70462314 | HCID 70462314 | 90% |
반응 단계
Mixed were 0.68 g of 7-ACA, 0.18 g of water and 0.90 g of 5-mercapto-2-morpholinocarbonylmethylthio-1,3,4-thiadiazole, and 4.0 ml of acetonitrile was added to the mixture, 2.52 g of diphosphoryl tetrachloride was added to the mixture under stirring in a dry ice/acetone bath at -20° to -40° C. over a period of about 10 minutes, and the cooling bath was removed. After the temperature was allowed to increase at 0° C., the reaction solution was stirred in a warm water bath at 40° C. for 20 minutes, cooled with ice and adjusted to pH 4.3 with aqueous concentrated ammonia following the addition of 5 ml of water. There was obtained 1.10 g (89.9% of yield) of 7-amino-3-(2-morpholinocarbonylmethylthio-1,3,4-thiadiazol-5-yl)thiomethyl-3-cephem-4-carboxylic acid thus produced.
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-fdc14065cefd49e48de1c3f236715201 |
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| 출처 메모 | uspto-grants-1984_05 |
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