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Potassium Phosphate, Tribasic → methyl 9-benzenesulfonyl-9H-[1,9']bicarbazolyl-1'-carboxylate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Potassium Phosphate, Tribasic | HCID 62657 | — |
| 反応物 | methyl 9H-carbazole-1-carboxylate | HCID 643304 | — |
| 反応物 | 9-(Benzenesulfonyl)-1-bromocarbazole | HCID 67405182 | — |
| 触媒 | Copper(1+) iodide; Copper(I) iodide; Cuprous iodide; Cuprous iodide (CuI) | HCID 24350 | — |
| 溶媒 | 1,4-Dioxane | HCID 31275 | — |
| 生成物 | methyl 9-benzenesulfonyl-9H-[1,9']bicarbazolyl-1'-carboxylate | HCID 68243195 | — |
反応手順
8.0 g (42.2 mmol) of copper(I) iodide, 11.7 ml (97.5 mmol) of trans-cyclo-hexanediamine are added to a well-stirred suspension of 26.3 g (117 mmol) of methyl 9H-carbazole-1-carboxylate, 45.2 g (117 mmol) of 9-benzenesulfonyl-1-bromo-9H-carbazole and 416.4 g (1961 mmol) of potassium phosphate in 1170 ml of dioxane, and the mixture is subsequently heated under reflux for 16 h. After cooling, the precipitated solid is filtered off with suction, washed three times with 50 ml of toluene, three times with 50 ml of ethanol:water (1:1, v:v) and three times with 100 ml of ethanol. Yield: 43 g (81 mmol), 70% of theory.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08835626B2 |
| 出典データセット | uspto-grants-2014_09 |
| ORD ID | ord-0c25fe28c9c74fb2ae1b964d5d9b0360 |
| 出典メモ | uspto-grants-2014_09 |