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Hydrochloric Acid → 3-(pyrazol-1-yl)-2-methyl-4-(methylsulfonyl)-N-(1-methyltetrazol-5-yl)benzamide
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | Thionyl Chloride | HCID 24386 | — |
| 反応物 | 1-methyl-1H-tetrazol-5-amine | HCID 138492 | — |
| 反応物 | 3-(Pyrazol-1-yl)-2-methyl-4-(methylsulfonyl)benzoic acid | HCID 66607037 | — |
| 触媒 | 4-(Dimethylamino)pyridine | HCID 14284 | — |
| 溶媒 | Water | HCID 962 | — |
| 溶媒 | Pyridine | HCID 1049 | — |
| 生成物 | 3-(pyrazol-1-yl)-2-methyl-4-(methylsulfonyl)-N-(1-methyltetrazol-5-yl)benzamide | HCID 66606785 | — |
反応手順
At RT, 178 mg (1.5 mmol) of thionyl chloride are added to 280 mg (1.0 mmol) of 3-(pyrazol-1-yl)-2-methyl-4-(methylsulfonyl)benzoic acid, 148 mg (1.5 mmol) of 1-methyl-5-aminotetrazole and 12 mg (0.1 mmol) of DMAP in 2 ml of pyridine. The mixture is stirred at RT for 12 h and, after having been checked by LCMS, stirred at 50° C. for 3 h. 0.1 ml of water is then added, the mixture is stirred at RT for 30 min and 2N HCl is added. The product is filtered off with suction and dried. Yield 134 mg (37%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08481749B2 |
| 出典データセット | uspto-grants-2013_07 |
| ORD ID | ord-26c8fb94f7d8496aacadce31e78043c7 |
| 出典メモ | uspto-grants-2013_07 |