関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Ethanol | HCID 702 | — |
| 反応物 | Dibenzothiophene | HCID 3023 | — |
| 反応物 | m-Chloroperbenzoic acid | HCID 70297 | — |
| 溶媒 | Chloroform | HCID 6212 | — |
| 生成物 | Dibenzothiophene sulfoxide | HCID 13898 | 76% |
反応手順
A solution of mCPBA (8.27 g, 36.9 mmol) in 71 mL chloroform was added dropwise over 30 minutes to a solution of dibenzothiophene in 89 mL chloroform at −35° C. The reaction mixture was stirred at −35° C. for 1 hour and then warmed up to room. The reaction was quenched with saturated sodium bicarbonate aqueous solution. The organic layer was washed with saturated sodium bicarbonate solution twice and dried over MgSO4, concentrated down to give an off-white solid. The solid was dissolved in refluxing ethanol and slowly cooled to room temperature to give a white crystalline solid Dibenzothiophene 5-oxide (5.65 g, 76%). LCMS-ESI−: calc'd for C12H8OS: 200.26. Found: 200.9 (M+H+).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08822430B2 |
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| 出典データセット | uspto-grants-2014_09 |
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| ORD ID | ord-4c5aa3ae301a45cd92a5eca7ac750ce3 |
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| 出典メモ | uspto-grants-2014_09 |
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