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Dibenzothiophene → 2-Bromodibenzothiophene
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Dibenzothiophene | HCID 3023 | — |
| 反応物 | Bromine | HCID 24408 | — |
| 反応物 | 2,8-Dibromodibenzothiophene | HCID 631120 | — |
| 反応物 | Sodium sulphite monohydrate | HCID 86645562 | — |
| 溶媒 | Chloroform | HCID 6212 | — |
| 生成物 | 2-Bromodibenzothiophene | HCID 299508 | — |
反応手順
15 g (79.9 mmol) dibenzothiophene was dissolved in 1.5 L chloroform. To the solution, 12.76 g (79.9 mmol) bromine was added dropwise. The reaction mixture was vigorously stirred for 2 days at room temperature and then treated with sodium sulfite water solution. The organic phase was evaporated to give a white solid which has 48% unreacted dibenzothiophene, 50% 2-bromodibenbzothiophene and ˜less 2% 2,8-dibromodibenzothiophene based on GC-MS and HPLC results. The mixture was repeatedly recrystallized with ethyl acetate to get pure 2-bromodibenzothiophene.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08822708B2 |
| 出典データセット | uspto-grants-2014_09 |
| ORD ID | ord-ffb5e1bcee37461ebd57d643b1d166a7 |
| 出典メモ | uspto-grants-2014_09 |