関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | 4-(2-Carboxyethyl)benzeneboronic acid | HCID 3863484 | — |
| 反応物 | Tert-butyl 3-(4-bromophenyl)propanoate | HCID 10708234 | — |
| 触媒 | HCID 178418397 | HCID 178418397 | — |
| 溶媒 | Ethyl Acetate | HCID 8857 | — |
| 溶媒 | Acetonitrile--water (1/1) | HCID 18373917 | — |
| 生成物 | tert-butyl 3-[4'-(2-Carboxy-ethyl)-biphenyl-4-yl]-propionate | HCID 66724435 | — |
反応手順
Tert-butyl 3-(4-bromophenyl)propionate (433 mg, 1.52 mmol) in acetonitrile-water (3:1, 13 ml) under argon atmosphere was treated with 4-(2-carboxyethyl)benzeneboronic acid (294 mg, 1.52 mmol), K2CO3 (251 mg, 1.82 mmol) and (Ph3P)4Pd (87 mg, 73 μmol), and the stirred mixture was heated at 90° C. for 4 hours. Excess ethyl acetate and 2 M HCl was added and the organic phase was washed with 2×2 M HCl and 2× water. Drying over MgSO4 and evaporation in vacuo gave the crude product, which was purified by chromatography on silica column eluted with ethyl acetate/hexane/acetic acid 50:50:1 to provide tert-butyl 3-[4′-(2-Carboxy-ethyl)-biphenyl-4-yl]-propionate, 330 mg (62%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US08067362B2 |
|---|
| 出典データセット | uspto-grants-2011_11 |
|---|
| ORD ID | ord-b816e92ded954250ad8daa17a66f86cd |
|---|
| 出典メモ | uspto-grants-2011_11 |
|---|
