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Sodium hydride → 1-[(5-Chloro-pyridin-2-ylcarbamoyl)-methyl]-1H-pyrazole-3,5-dicarboxylic acid diethyl ester
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Sodium hydride | HCID 24758 | — |
| 反応物 | diethyl 1H-pyrazole-3,5-dicarboxylate | HCID 142184 | — |
| 反応物 | 2-Bromo-N-(5-chloro-2-pyridinyl)acetamide | HCID 3421110 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | 1-[(5-Chloro-pyridin-2-ylcarbamoyl)-methyl]-1H-pyrazole-3,5-dicarboxylic acid diethyl ester | HCID 60207957 | — |
反応手順
To a solution of 10 g 1H-Pyrazole-3,5-dicarboxylic acid diethyl ester in 200 ml absolute DMF 1.885 g of a 60% suspension of NaH in mineral oil were added in an argon atmosphere. The mixture was stirred for 15 min at RT. 11.76 g 2-Bromo-N-(5-chloro-pyridin-2-yl)-acetamide were added and the mixture stirred for 2 h at RT. After concentration in vacuo the residue was purified by chromatography on silica gel using CH2Cl2/ethylacetate=8/2. The fractions containing the product were evaporated. Yield: 16.05 g.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07429581B2 |
| 出典データセット | uspto-grants-2008_09 |
| ORD ID | ord-e88c35d032e04b21ac5ba4ec27b8a34a |
| 出典メモ | uspto-grants-2008_09 |