関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Nitric Acid | HCID 944 | — |
| 反応物 | Ammonium Hydroxide | HCID 14923 | — |
| 反応物 | HNO3 dichloromethane | HCID 20264123 | — |
| 反応物 | N-(4-(Oxetan-3-YL)phenyl)acetamide | HCID 67776166 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | N-(2-nitro-4-(oxetan-3-yl)phenyl)acetamide | HCID 67776164 | — |
反応手順
The organic phase (upper phase) was isolated and the process was repeated with an additional 20 ml CH2Cl2. The organic extracts were combined, it was assumed the organic phase contained about 5 g (−80 mmol) of anhydrous HNO3. Using a 50 fold excess, this required about 25 ml of solution. The nitric acid solution was cooled in a ice bath. The N-(4-oxetan-3-ylphenyl)acetamide (21 0 mg, 0.70 mmol) was treated with 25 ml of the chilled HNO3/CH2Cl2 solution and was allowed to stir about 30 minutes. The reaction mixture was carefully poured into 45 ml 1 0% NH4OH solution and carefully shaken. The phases were separated and the aqueous phase was washed with 20 ml CH2Cl2. The combined organic phase was dried over Na2SO4, filtered and concentrated. The crude material was purified
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US09096634B2 |
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| 出典データセット | uspto-grants-2015_08 |
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| ORD ID | ord-e1917049c81346c38e02a6ec24682373 |
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| 出典メモ | uspto-grants-2015_08 |
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