関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Dimethylformamide | HCID 6228 | — |
| 反応物 | Ethanedioyl dibromide | HCID 84841 | — |
| 反応物 | methyl 4-chloro-3-(2,3-dioxo-3,4-dihydropyrazin-1(2H)-yl)benzoate | HCID 66690376 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | methyl 3-(3-bromo-2-oxopyrazin-1(2H)-yl)-4-chlorobenzoate | HCID 66689444 | — |
反応手順
A suspension of methyl 4-chloro-3-(2,3-dioxo-3,4-dihydropyrazin-1(2H)-yl)benzoate (Example 330d, 8 g) in DCM (80 mL) was treated with N,N-dimethylformamide (0.220 mL) and oxalyl bromide (2.94 mL) dropwise over 5 min at room temperature under nitrogen. The resulting mixture was stirred at 20° C. for 16 h. The reaction mixture turned black and was evaporated to afford crude product. Purification (SiO2 chromatography eluting with 30% diethyl ether in dichloromethane) gave the subtitle compound (6.33 g).
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-271e63ae36d64fd78b65832e5789dbc4 |
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| 出典メモ | uspto-grants-2014_11 |
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