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 resultant crude protected ampicillin mixture is worked up by treating with a mixture of 289 ml ice-water and 39.6 ml concentrated HCl and stirred for 30 minutes while cooling with ice. The aqueous phase is separated off and the organic phase back-extracted with a mixture of 5.4 ml concentrated HCl and 44.5 ml water. The combined aqueous phases are filtered through a filtering aid and pumped into a suspension of 5 g ampicillin trihydrate seed crystals in 100 ml water keeping the pH from 4.5 to 5.0 by the addition of concentrated aqueous ammonia. The title compound is obtained by standing the mixture overnight in a refrigerator, isolating the crystals, and washing them with 60 ml ice-water and 3×50 ml 90% acetone, followed by drying. Yield 61.6 g=82.4%, Purity 98.8%.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US05840885 |
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| 出典データセット | uspto-grants-1998_11 |
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| ORD ID | ord-751273514a5d4d02b8be4f0496d72038 |
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| 出典メモ | uspto-grants-1998_11 |
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