関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Nitrogen | HCID 947 | — |
| 反応物 | 1,10-Phenanthroline | HCID 1318 | — |
| 反応物 | 1-tert-Butyl-4-iodobenzene | HCID 142029 | — |
| 反応物 | 2,7-Dibromocarbazole | HCID 11151503 | — |
| 触媒 | Cuprous chloride | HCID 62652 | — |
| 溶媒 | Water | HCID 962 | — |
| 溶媒 | Toluene | HCID 1140 | — |
| 生成物 | N-(4-tert-Butylphenyl)-2,7-dibromocarbazole | HCID 59557277 | — |
反応手順
A degassed solution of 489.5 mg (0.156%) of copper(I) chloride and 906 mg (1%) mmol) of 1,10-phenanthroline in 100 ml of toluene were saturated with N2 for 1 hour and heated to 130° C. The solution was subsequently admixed with 16.2 g (50 mmol) of 2,7-dibromocarbazole and 13.2 g (50 mmol) of 1-iodo-4-tert-butylbenzene and heated at 180° C. for 2 hours. After cooling, the mixture was admixed with 180 ml of water, the organic phase was separated off and the solvent was removed under reduced pressure. The product was recrystallized from n-hexane. Yield: 13 g (59%). Purity according to HPLC: 99.5%
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US08053547B2 |
|---|
| 出典データセット | uspto-grants-2011_11 |
|---|
| ORD ID | ord-5d278e7e266b4969a7763f8bd154691b |
|---|
| 出典メモ | uspto-grants-2011_11 |
|---|
