関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Phenol | HCID 996 | — |
| 反応物 | 1,4-Cyclohexadiene | HCID 12343 | — |
| 反応物 | Diisopropylethylamine | HCID 81531 | — |
| 反応物 | methyl 3-(3,5-dibromo-2-oxopyrazin-1(2H)-yl)-4-methylbenzoate | HCID 66688740 | — |
| 触媒 | Palladium | HCID 23938 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | 4-Methyl-3-(2-oxo-3-phenoxy-1(2H)-pyrazinyl)-benzoic acid, methyl ester | HCID 86663239 | — |
反応手順
A mixture of 3-(3,5-dibromo-2-oxo-2H-pyrazin-1-yl)-4-methyl-benzoic acid, methyl ester (Example 1b, 400 mg), phenol (400 mg), N,N-diisopropylethylamine (0.4 mL) and tetrahydrofuran (2 mL) was heated within a microwave for 3 h at 120° C. before being cooled to room temperature. The mixture was transferred to a mixture of palladium on carbon (10%, 38 mg) and tetrahydrofuran (1 mL). 1,4-Cyclohexadiene (2 mL) was added and the mixture was heated under atmosphere of nitrogen within a microwave for 15 minutes at 90° C. before being cooled to room temperature. The mixture was filtered and concentrated to give a crude product that was used in the next step without purification.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08889692B2 |
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| 出典データセット | uspto-grants-2014_11 |
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| ORD ID | ord-772973e7b197498ab8a77ab4301a1b29 |
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| 出典メモ | uspto-grants-2014_11 |
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