関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | Sodium Carbonate | HCID 10340 | — |
| 反応物 | 2-(4-(4,4,5,5-Tetramethyl-1,3,2-dioxaborolan-2-yl)phenyl)acetic Acid | HCID 3719002 | — |
| 反応物 | HCID 66750884 | HCID 66750884 | — |
| 触媒 | HCID 178418397 | HCID 178418397 | — |
| 溶媒 | Toluene | HCID 1140 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 溶媒 | Ethanol ethylacetate | HCID 21584252 | — |
| 生成物 | HCID 66751287 | HCID 66751287 | 26.4% |
反応手順
A mixture of 1-[(4-bromophenyl)carbonyl]-4-(2-tert-butylphenyl)piperazine (1.0 g, 2.49 mmol), [4-(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl)phenyl]acetic acid (0.653 g, 2.49 mmol), 2 M sodium carbonate solution (3 mL, 6.0 mmol), and tetrakis(triphenylphosphine)palladium(0) (0.150 g, 0.13 mmol) in tetrahydrofuran (5 mL) and toluene (20 mL) was stirred at 120° C. for 16 h. 6 M hydrochloric acid solution was added and the mixture was extracted with ethyl acetate. The organic layer was washed with brine, dried over anhydrous magnesium sulfate, filtered and concentrated under reduced pressure to afford a solid. The solid was dissolved in ethanol-ethyl acetate and recrystallized to obtain a solid (0.3 g, 26%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US08853215B2 |
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| 出典データセット | uspto-grants-2014_10 |
|---|
| ORD ID | ord-728f5dec0c8547e88c4584c694190c2e |
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| 出典メモ | uspto-grants-2014_10 |
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