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Potassium Phosphate, Tribasic → 9-Biphenyl-2-ylbenzo[4,5]imidazo[2,1-a]isoquinoline
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Potassium Phosphate, Tribasic | HCID 62657 | — |
| 反応物 | Tri-o-tolylphosphine | HCID 80271 | — |
| 反応物 | Biphenyl-2-boronic acid | HCID 4589187 | — |
| 反応物 | 9-Bromobenzimidazo[2,1-a]isoquinoline | HCID 71077841 | — |
| 触媒 | palladium(II) acetate | HCID 167845 | — |
| 溶媒 | Water | HCID 962 | — |
| 溶媒 | Toluene | HCID 1140 | — |
| 溶媒 | 1,4-Dioxane | HCID 31275 | — |
| 生成物 | 9-Biphenyl-2-ylbenzo[4,5]imidazo[2,1-a]isoquinoline | HCID 71077930 | — |
反応手順
913 mg (3 mmol) of tri-o-tolylphosphine and then 112 mg (0.5 mmol) of palladium(II) acetate are added to a vigorously stirred suspension of 14.8 g (50 mmol) of 9-bromobenzimidazo[2,1-a]isoquinoline, 9.9 g (55 mmol) of 1,1′-biphenyl-2-boronic acid and 25.5 g (120 mmol) of tri-potassium phosphate in a mixture of 300 ml of toluene, 100 ml of dioxane and 400 ml of water, 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), three times with 100 ml of ethanol and finally dried. The residue is recrystallised from toluene. The yield is 17 g (45 mmol, 92%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US09118022B2 |
| 出典データセット | uspto-grants-2015_08 |
| ORD ID | ord-30f4b6e632154c02baa0cf9d66528242 |
| 出典メモ | uspto-grants-2015_08 |