関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | Methanol | HCID 887 | — |
| 反応物 | Sodium Methoxide | HCID 10942334 | — |
| 反応物 | 4-Desmethoxy-4-chloro Omeprazole Sulfide | HCID 178488122 | — |
| 溶媒 | Ethyl Acetate | HCID 8857 | — |
| 生成物 | HCID 178488125 | HCID 178488125 | 85% |
反応手順
First, 277 mg (0.92 mmol) of 5-methoxy-2-{[(4-chloro-3,5-dimethyl-2-pyridyl)methyl]thio}-1H-benzimidazole obtained in Example 21 and 1.00 g (5.20 mmol) of methanol 28% solution of sodium methoxide were introduced to a 3-necked flask (30 ml volume) equipped with a thermometer, a magnetic stirrer and a condenser tube, and the mixture was agitated for 10 hours while being slowly refluxed. Then the mixture was neutralized with dilute hydrochloric acid. Ethyl acetate (10 ml) was added thereto and an organic layer was separated, and an aqueous layer was extracted twice with 10 ml of ethyl acetate. The extracts and the above mentioned organic layer were combined and dried over anhydrous magnesium sulfate. The solvent was removed under reduced pressure to give 232 mg of 5-methoxy-2-{[(4-methoxy-3,5-dimethyl-2-pyridyl)methyl]thio}-1H-benzimidazole (yield of 85%) with revealing the properties.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US06350876B2 |
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| 出典データセット | uspto-grants-2002_02 |
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| ORD ID | ord-4b5b552b356c4355b7ec698af979dc80 |
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| 出典メモ | uspto-grants-2002_02 |
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