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4-Aminobenzoic Acid → 4-(4-(1-(2-cyano-1-cyclopropylethyl)-1H-pyrazol-4-yl)pyrimidin-2-ylamino)benzoic Acid
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 4-Aminobenzoic Acid | HCID 978 | — |
| 反応物 | p-Toluenesulfonic acid | HCID 6101 | — |
| 反応物 | 3-(4-(2-chloropyrimidin-4-yl)-1H-pyrazol-1-yl)-3-cyclopropylpropanenitrile | HCID 86637293 | — |
| 溶媒 | 1,4-Dioxane | HCID 31275 | — |
| 生成物 | 4-(4-(1-(2-cyano-1-cyclopropylethyl)-1H-pyrazol-4-yl)pyrimidin-2-ylamino)benzoic Acid | HCID 58014454 | — |
反応手順
A mixture of 3-(4-(2-chloropyrimidin-4-yl)-1H-pyrazol-1-yl)-3-cyclopropylpropanenitrile (2.74 g, 0.0100 mol), p-aminobenzoic acid (2.06 g, 0.0150 mol), and p-toluenesulfonic acid (1.5 g, 0.0085 mol) in dry 1,4-dioxane (80 mL) was refluxed overnight. The mixture was cooled to room temperature, filtered. The solid was washed with dioxane, air dried to yield the desired product as a racemic mixture (3.02 g, 80.58%). LCMS (M+H) 375.3.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08309718B2 |
| 出典データセット | uspto-grants-2012_11 |
| ORD ID | ord-26f869aef9204275bb308e478280a5aa |
| 出典メモ | uspto-grants-2012_11 |