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Hydrochloric Acid → 4,7-dihydro-1,6-dimethyl-3-phenyl-4-(2-methylphenyl)-1H-pyrazolo[3,4-b]pyridin-5-carboxylic acid ethyl ester, hydrochloride
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | Methanol | HCID 887 | — |
| 反応物 | 1-Methyl-3-phenyl-1H-pyrazol-5-amine | HCID 517779 | — |
| 反応物 | Ethyl-2-(2-methylbenzyliden)acetoacetate | HCID 54239661 | — |
| 溶媒 | Ethanol | HCID 702 | — |
| 生成物 | 4,7-dihydro-1,6-dimethyl-3-phenyl-4-(2-methylphenyl)-1H-pyrazolo[3,4-b]pyridin-5-carboxylic acid ethyl ester, hydrochloride | HCID 137225460 | — |
反応手順
Ethyl-2-(2-methylbenzyliden)acetoacetate (0.050 mol) is added to 1-methyl-3-phenyl-5-pyrazolamine (0.050 mol) in ethanol (50 ml) and refluxed for 90 minutes. The mixture is then cooled to room temperature, further ethyl-2-(2-methylbenzyliden)acetoacetate (0.050 mol) is added thereto, and the mixture refluxed for further 90 minutes. The reaction mixture is then cooled, the solvent is evaporated, and the residue is taken up in ethyl ether, collected by filtration, and dried. The product is dissolved in methanol and a mixture of hydrochloric acid and methanol (45 mmol of HCl) is added thereto. The product of the title precipitates by adding ethyl ether. M.p. 187° C. (dec.).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04954508 |
| 出典データセット | uspto-grants-1990_09 |
| ORD ID | ord-a78c6a8330e642d08d1e3b3b76774091 |
| 出典メモ | uspto-grants-1990_09 |