関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | Methyl chloroglyoxylate | HCID 79846 | — |
| 反応物 | 6-Chloro-4-(isopropylamino)nicotinohydrazide | HCID 89689668 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | Methyl 2-(2-(6-chloro-4-(isopropylamino)nicotinoyl)hydrazinyl)-2-oxoacetate | HCID 89689816 | — |
反応手順
To a stirred solution of 6-chloro-4-(isopropylamino)nicotinohydrazide (10) (200 mg, 0.35 mmol) in DCM (10 mL), Et3N (3.1 mmol, 3 equiv) was added and cooled to 0° C. Methyl 2-chloro-2-oxoacetate (0.42 mmol, 1.2 equiv) was added dropwise and stirred for 6 h at room temperature. The reaction mixture was quenched with aq. NaHCO3 solution and extracted in DCM. The organic layer was separated, dried over Na2SO4, filtered and concentrated. The crude material was purified by column chromatography through silica gel and MeOH: DCM as eluent to afford methyl 2-(2-(6-chloro-4-(isopropylamino)nicotinoyl)hydrazinyl)-2-oxoacetate.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08987311B2 |
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| 出典データセット | uspto-grants-2015_03 |
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| ORD ID | ord-45185bd5531d4c0094c07877bc2ded5b |
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| 出典メモ | uspto-grants-2015_03 |
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