関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Sodium Hydroxide | HCID 14798 | — |
| 反応物 | Sodium Sulfite | HCID 24437 | — |
| 反応物 | Omeprazole sulfide | HCID 155794 | — |
| 反応物 | Potassium Bicarbonate | HCID 516893 | — |
| 反応物 | Monoperoxyphthalic Acid Magnesium Salt | HCID 10130449 | — |
| 溶媒 | Ethanol | HCID 702 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 溶媒 | Water | HCID 962 | — |
| 溶媒 | Toluene | HCID 1140 | — |
| 生成物 | HCID 178488147 | HCID 178488147 | 81% |
反応手順
A mixture of pyrmetazole (0.112 mole) and potassium bicarbonate (0.145 mole) in 100 mL of water and approximately 250 mL of a 4:1; toluene: ethanol mixture was cooled to -5° to -9° C. with stirring. A solution of MMPP (0.67 mol) in 170 mL of water was added dropwise over a 2 hour period. After the MMPP solution was completely added a solution of sodium sulfite (2.2g) in 10 mL of water was added and the mixture was stirred for 15 minutes. The reaction mixture temperature was allowed to warm to 0° C. during this period. The slurry was then diluted with 200 mL of water and 50 mL of methanol and the pH of the slurry was adjusted to 9.1 by addition of 50% aqueous sodium hydroxide. The slurry was aged at 0° to 5° C. for 1 hour and then was filtered. The solid was washed with 50 mL of water and 40 mL cold methanol. Drying of the solid provided 31.3 g of crude omeprazole (81% yield).
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 |
|---|
| ORD ID | ord-b6a15d6f76b6457697cb9df2e62aa10d |
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| 出典メモ | uspto-grants-1995_02 |
|---|