関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | Ampicillin | HCID 6249 | — |
| 生成物 | Ampicillin Trihydrate | HCID 23565 | — |
反応手順
The mixture obtained in step a) is added dropwise to the mixture obtained in step b) at a temperature of -45/-35°. The resultant mixture is stirred for 2 hours at a temperature of -15/-35°. The resultant crude protected ampicillin mixture is worked up by treating with a mixture of ice-water and concentrated hydrochloric acid and stirred for 20 minutes while cooling with ice. The aqueous phase is separated off and the organic phase is reextracted with a mixture of water and concentrated hydrochloric acid. The combined aqueous phases are treated with concentrated aqueous sodium hydroxide to a pH of 4.5/5.5. Ampicillin trihydrate crystallizes out of the reaction mixture overnight in a refrigerator, the crystals are isolated, washed with IPA 88% and dried. Yield 89.0%, Purity 98.4%.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US05998610 |
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| 出典データセット | uspto-grants-1999_12 |
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| ORD ID | ord-29d57cd435354d7bbcdd88b43453a9d6 |
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| 出典メモ | uspto-grants-1999_12 |
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