関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | 1-Bromo-4-iodobenzene | HCID 11522 | — |
| 反応物 | 4-(Diphenylamino)phenylboronic Acid (contains varying amounts of Anhydride) | HCID 12166934 | — |
| 触媒 | HCID 178418397 | HCID 178418397 | — |
| 溶媒 | 1,4-Dioxane--water (1/1) | HCID 21886435 | — |
| 生成物 | 4-Bromo-4'-(diphenylamino)biphenyl | HCID 11315550 | — |
反応手順
A mixture of 4-diphenylaminophenyl boronic acid (2.57 g, 8.9 mmol), 4-bromo-iodobenzene (5.03 g, 17.8 mmol), Pd(PPh3)4 (0.58 g, 0.5 mmol) and K2CO3 (3.0 g, 22 mmol) in dioxane/water (80 mL/15 mL) was degassed and heated at about 80° C. for about 20 hours. The whole was mixed with water/dichloromethane, the organic phase was collected and washed with brine, dried over Na2SO4, loaded on silica gel, and purified by flash column (hexanes to hexanes/dichloromethane 30:1). The desired fraction was collected, and concentrated to give a white solid (Compound 12), which was filtered and washed with methanol (2.70 g, in 76% yield).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US09172051B2 |
|---|
| 出典データセット | uspto-grants-2015_10 |
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| ORD ID | ord-86bb1e26cedb4b5fbe2e4158e2bf52ec |
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| 出典メモ | uspto-grants-2015_10 |
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