関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | Ethanol | HCID 702 | — |
| 反応物 | 7-Aminodeacetoxycephalosporanic acid | HCID 33498 | — |
| 反応物 | Sodium Nitrite | HCID 23668193 | — |
| 溶媒 | Water | HCID 962 | — |
| 溶媒 | Sodium chloride; water | HCID 57417360 | — |
| 生成物 | 7alpha-Chloro-3-methyl-3-cephem-4-carboxylic acid | HCID 15660493 | — |
反応手順
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.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US05264430 |
|---|
| 出典データセット | uspto-grants-1993_11 |
|---|
| ORD ID | ord-4f66a560b4d744959a2551b9024d02ec |
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| 出典メモ | uspto-grants-1993_11 |
|---|
