関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 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 | Chloroform | HCID 6212 | — |
| 生成物 | S-Methyl-S-(4-nitrophenyl)sulfoximine | HCID 12463933 | — |
反応手順
23.65 g (127.7 mmol) (RS)-1-(methylsulfinyl)-4-nitrobenzene in 130 ml chloroform are treated with 9.32 g (143.4 mmol) sodium azide. The mixture is slowly treated with 32.4 ml of concentrated sulfuric acid at 0° C. and then slowly heated to 45° C. After 16 hrs, the mixture is cooled to room temperature, treated with ice-water and extracted with chloroform. This organic phase is discarded. The aqueous phase is basified with 2N NaOH solution and extracted with DCM. The combined organic phases are washed with saturated NaCl solution, dried (Na2SO4), filtered and concentrated. 17.17 g (88.4 mmol, corresponding to 63% of theor.) of the product is obtained.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08524724B2 |
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| 出典データセット | uspto-grants-2013_09 |
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| ORD ID | ord-692fa87441cb477a8e2d3081c0f0bc96 |
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| 出典メモ | uspto-grants-2013_09 |
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