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Diethyl Ether → 1h-Indazole-1-carboxylic acid,5-(azidomethyl)-3-(3-fluorophenyl)-,1,1-dimethylethyl ester
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Diethyl Ether | HCID 3283 | — |
| 反応物 | Sodium Azide | HCID 33557 | — |
| 反応物 | 1h-Indazole-1-carboxylic acid,5-(chloromethyl)-3-(3-fluorophenyl)-,1,1-dimethylethyl ester | HCID 22260616 | — |
| 溶媒 | Dimethyl Sulfoxide | HCID 679 | — |
| 生成物 | 1h-Indazole-1-carboxylic acid,5-(azidomethyl)-3-(3-fluorophenyl)-,1,1-dimethylethyl ester | HCID 22260873 | 93.5% |
反応手順
To a solution of 600 mg of tert-butyl 5-(chloromethyl)-3-(3-fluorophenyl)-1H-1-indazolecarboxylate produced in Production Example I-24-b in 4 ml dimethyl sulfoxide was added 162 mg of sodium azide, and the mixture was stirred at room temperature for 50 minutes. To the reaction mixture was added 25 ml of diethyl ether. The mixture was sequentially washed with water (×3) and brine, dried over anhydrous magnesium sulfate and the solvent was evaporated, to give 571 mg of the title compound as pale yellow crystals.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06982274B2 |
| 出典データセット | uspto-grants-2006_01 |
| ORD ID | ord-bea9cff08ac74da6afc8b9a20ea6da97 |
| 出典メモ | uspto-grants-2006_01 |