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HRID 496596作成日:2026年10月26日
Potassium Carbonate → Ethyl 4-[(4-fluorobenzenesulfonyl)methylamino]-1,3-dimethyl-1h-pyrazolo[3,4-b] pyridine-5-carboxylate
https://huagongshe.com/reaction/496596
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | N-methyl-2-pyrrolidone | HCID 13387 | — |
| 反応物 | 4-fluoro-N-methylbenzene-1-sulfonamide | HCID 2440054 | — |
| 反応物 | ethyl 4-chloro-1,3-dimethyl-1H-pyrazolo[3,4-b]pyridine-5-carboxylate | HCID 2736380 | — |
| 触媒 | 18-Crown-6 | HCID 28557 | — |
| 生成物 | Ethyl 4-[(4-fluorobenzenesulfonyl)methylamino]-1,3-dimethyl-1h-pyrazolo[3,4-b] pyridine-5-carboxylate | HCID 69733699 | — |
反応手順
A mixture of 2.53 g (0.01 mol) of ethyl 4-chloro-1,3-dimethyl-1H pyrazolo[3,4-b]pyridine-5-carboxylate, 1.89 g (0.01 mol) of N-methyl-4-fluorobenzenesulfonamide, 6.91 g (0.05 mol) of anhydrous K2CO3, 0.143 g of 18-crown-6 and 70 ml of anhydrous 1-methyl-2-pyrrolidinone was stirred and heated at 100° C. for 17 hours. The solvent was removed under vacuum and water added to the residue. The mixture was extracted with CH2Cl2, and the extract washed with H2O, brine and dried (Na2SO4). The solution was filtered through a pad of hydrous magnesium silicate and the filtrate concentrated to dryness under vacuum to give 4.98 g of an oil. This oil was chromatographed on a silica gel column with ethyl acetate-hexane(2:3) as solvent to give 3.15 g of solid, mp 107-109° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US06946473B2 |
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| 出典データセット | uspto-grants-2005_09 |
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| ORD ID | ord-4b82875573834294837352ec2141a354 |
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| 出典メモ | uspto-grants-2005_09 |
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