참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Hydrochloric Acid | HCID 313 | — |
| 반응물 | Ethanol | HCID 702 | — |
| 반응물 | 7-Aminodeacetoxycephalosporanic acid | HCID 33498 | — |
| 반응물 | Sodium Nitrite | HCID 23668193 | — |
| 용매 | Water | HCID 962 | — |
| 용매 | Sodium chloride; water | HCID 57417360 | — |
| 생성물 | 7alpha-Chloro-3-methyl-3-cephem-4-carboxylic acid | HCID 15660493 | — |
반응 단계
A mixture of 7-ADCA (25 g, 0.117 mol), ethanol (700 ml), water (163 ml) and concentrated hydrochloric acid (163 ml) was cooled to 5° C. Sodium nitrite (11.5 g, 0.167 mol) was added in small portions over 25 minutes and the mixture was stirred for 3.5 hours at 0°-5° C.; 300 ml of brine was added and the reaction mixture was extracted with methylene chloride. The organic extract was washed with water, brine, dried over sodium sulfate and concentrated (16.1 g, 58.9%). This crude acid was directly used for the next step without further purification.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 특허 번호 | US05264430 |
|---|
| 출처 데이터셋 | uspto-grants-1993_11 |
|---|
| ORD ID | ord-4f66a560b4d744959a2551b9024d02ec |
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| 출처 메모 | uspto-grants-1993_11 |
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