関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | Sulfuric Acid | HCID 1118 | — |
| 反応物 | Sodium Azide | HCID 33557 | — |
| 反応物 | 1-(Methylsulfinyl)-4-nitrobenzene | HCID 305882 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | S-Methyl-S-(4-nitrophenyl)sulfoximine | HCID 12463933 | 63% |
反応手順
0.70 g (10.76 mmol) of sodium azide was added to 1.56 g (8.42 mmol) of 1-(methylsulfinyl)-4-nitrobenzene in 20 ml DCM. 2.3 ml concentrated sulfuric acid was slowly added to the mixture at 0° C. and it was then heated to 45° C. After 16 h the mixture was cooled to room temperature, and after adding water it was extracted with DCM. The aqueous phase was adjusted to pH 11 with 15% sodium hydroxide solution and extracted with DCM (2×). The combined organic phases were dried (Na2SO4), filtered and concentrated by evaporation. 1.08 g (5.39 mmol; yield: 63%) of the product was obtained.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08735412B2 |
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| 出典データセット | uspto-grants-2014_05 |
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| ORD ID | ord-b10c2abfd46341f98010011db5af47d9 |
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| 出典メモ | uspto-grants-2014_05 |
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