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4-benzenesulphonyl-5-methylsulphanyl-2H-pyrazol-3-ylamine → HCID 178494547、化合物
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 4-benzenesulphonyl-5-methylsulphanyl-2H-pyrazol-3-ylamine | HCID 11054717 | — |
| 反応物 | Ethyl 4-methoxy-3-oxobutanoate | HCID 12645099 | — |
| 溶媒 | Acetic Acid | HCID 176 | — |
| 生成物 | HCID 178494547 | HCID 178494547 | 85% |
反応手順
A solution of 2.69 g (10 mmol) 4-benzenesulphonyl-5-methylsulphanyl-2H-pyrazol-3-ylamine and 1.46 g (10 mmol) of ethyl 4-methoxy-acetoacetate in 10 ml of acetic acid was heated at reflux for 3 hrs. The reaction solution was evaporated and the residue was partitioned between H2O and CH2Cl2. The aqueous phase was extracted three times with 80 ml of CH2Cl2. The combined organic phases were dried (MgSO4), filtered and evaporated. Chromatography (SiO2, CH2Cl2/MeOH 25:1) yielded 3.1 g (85%) of 3-benzenesulphonyl-5-methoxymethyl-2-methylsulphanyl-pyrazolo[1,5-a]pyrimidin-7-ol as a beige powder, m.p. 175-155°.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06194410B1 |
| 出典データセット | uspto-grants-2001_02 |
| ORD ID | ord-71c13a4487e84535bdbd8749a6661bb8 |
| 出典メモ | uspto-grants-2001_02 |