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Diisopropylethylamine → HCID 57378953、化合物
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Diisopropylethylamine | HCID 81531 | — |
| 反応物 | Propylphosphoric anhydride | HCID 16167369 | — |
| 反応物 | 4-(Methoxycarbonyl)-1-methyl-1H-pyrazole-5-carboxylic acid | HCID 45923681 | — |
| 反応物 | 2-Phenyl-[1,2,4]triazolo[1,5-a]pyridin-7-ylamine | HCID 67774145 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 溶媒 | Sodium Bicarbonate | HCID 516892 | — |
| 生成物 | HCID 57378953 | HCID 57378953 | 94.5% |
反応手順
A solution of 2-phenyl-[1,2,4]triazolo[1,5-a]pyridin-7-ylamine (1.534 g, 7.3 mmol), 4-(methoxycarbonyl)-1-methyl-1H-pyrazole-5-carboxylic acid (1.61 g, 8.76 mmol), propylphosphonic anhydride (50% in ethyl acetate, 10.7 ml, 18.2 mmol) and diisopropylethylamine (5.1 ml, 29.2 mmol) in tetrahydrofurane (54 ml) is stirred at 70° C. for 1.25 hr giving a white suspension. The cooled suspension is poured in sat. aqueous sodium bicarbonate solution (200 ml), stirred at room temperature for 15 min and the solid is collected by filtration, washed with water and dried affording methyl 1-methyl-5-(2-phenyl-[1,2,4]triazolo[1,5-a]pyridin-7-ylcarbamoyl)-1H-pyrazole-4-carboxylate (2.596 g, 94.5%) as a white solid. mp.: 243-7° C. MS: m/z=377.2 (M+H+).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08349824B2 |
| 出典データセット | uspto-grants-2013_01 |
| ORD ID | ord-855055d4ec904c1a96d094e383d2d916 |
| 出典メモ | uspto-grants-2013_01 |