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 | (4-Chloro-2-methoxyphenyl)boronic acid | HCID 3858606 | — |
| 反応物 | Methyl [3-bromo-4-(3-fluorobenzyl)-5-oxo-4,5-dihydro-1H-1,2,4-triazol-1-yl]-acetate | HCID 58011964 | — |
| 触媒 | HCID 178418397 | HCID 178418397 | — |
| 生成物 | HCID 58011821 | HCID 58011821 | — |
反応手順
Under argon, 250 mg (0.73 mmol) of the compound from Example 146A and 190 mg (1.07 mmol) of 4-chloro-2-methoxyphenylboronic acid are dissolved in 7 ml degassed DMF. A previously degassed solution of sodium carbonate (2 N in water, 1.09 ml, 2.18 mmol) and 42 mg of tetrakis(triphenylphosphine)palladium (0.036 mmol) are added. The resulting mixture is heated and stirred for 8 hrs at 90° C. After cooling to RT it is acidified with 10% hydrochloric acid and the mixture filtered. The filtrate is purified by preparative HPLC (Method 20). 159 mg (54% of theory) of the title compound and 54 mg (18% of theory) of the corresponding acid formed by hydrolysis (see also Example 148A) are obtained.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US08084481B2 |
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| 出典データセット | uspto-grants-2011_12 |
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| ORD ID | ord-d52fe195bdb241f4b0f9df181d8252d5 |
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| 出典メモ | uspto-grants-2011_12 |
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