関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Omeprazole sulfide | HCID 155794 | — |
| 反応物 | Sodium Bicarbonate | HCID 516892 | — |
| 反応物 | Monoperoxyphthalic Acid Magnesium Salt | HCID 10130449 | — |
| 反応物 | Methanol--water (1/1) | HCID 22242641 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | HCID 178488147 | HCID 178488147 | 92% |
反応手順
To a solution of 3.44 g of pyrmetazole (10.5 mmol) in 30 mL of 9:1 v/v methanol/water at -10° C. was added dropwise a solution of 3.10 g of MMPP in 30 mL of 9:1 v/v methanol/water over a 10 minute period. The reaction mixture was stirred at -10° C. for 35 minutes then poured into a mixture of 100 mL of saturated aqueous sodium bicarbonate and 40 mL of methylene chloride. The layers were separated and the aqueous layer was extracted 3 times with methylene chloride. The combined organic layers were dried over anhydrous magnesium sulfate and filtered. The filtrate was concentrated under vacuum and the residue was slurried in EtOAc and the slurry stirred for 10 minutes. The solid was collected and then dried to provide 3.31 g of omeprazole (92% yield). LC analysis showed that the product was 99.5% pure.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US05391752 |
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| 出典データセット | uspto-grants-1995_02 |
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| ORD ID | ord-22f30f4e398e46bb82be0430fa6320ff |
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| 出典メモ | uspto-grants-1995_02 |
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