関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Sodium hydride | HCID 24758 | — |
| 反応物 | 2-Iodobenzene-1-sulfonyl chloride | HCID 627400 | — |
| 反応物 | 1-Bromo-9H-carbazole | HCID 11230335 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | 9-(Benzenesulfonyl)-1-bromocarbazole | HCID 67405182 | — |
反応手順
19.6 g (80 mmol) of 1-bromocarbazole are initially introduced in 1000 ml of THF, and 8.9 g (223.3 mmol) of NaH (60% in oil) are added at 0° C. 24 g (80 mmol) of 2-iodobenzenesulfonyl chloride are subsequently added to the mixture, which is then stirred at 40° C. for 12 h. The organic phase is dried over MgSO4, and the solvent is removed in vacuo. The residue is recrystallised from acetone and finally sublimed in a high vacuum. Yield: 29 g (574 mmol), 72% of theory, purity according to HPLC 99.9%.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US08835626B2 |
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| 出典データセット | uspto-grants-2014_09 |
|---|
| ORD ID | ord-3c43d7a676ae43afb3bbd4062c96f588 |
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| 出典メモ | uspto-grants-2014_09 |
|---|
