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Benzyl chloroformate → Benzyl (S)-2-(6-hydroxy-1H-indazol-1-yl)-1-methylethylcarbamate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Benzyl chloroformate | HCID 10387 | — |
| 反応物 | Sodium Bicarbonate | HCID 516892 | — |
| 反応物 | AL-34662 | HCID 135453290 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | Benzyl (S)-2-(6-hydroxy-1H-indazol-1-yl)-1-methylethylcarbamate | HCID 135487328 | 78% |
反応手順
1-((S)-2-Aminopropyl)-1H-indazol-6-ol [prepared in accordance with commonly owned WO 02/098862A1, the contents of which are by this reference incorporated herein] (2.00 g, 10.5 mmol) was suspended in THF (20 mL) and saturated aqueous sodium bicarbonate (10 mL) and benzyl chloroformate (1.50 mL, 15 mol) were added. The mixture was stirred at room temperature until the starting amine dissolved. Saturated aqueous sodium bicarbonate (150 mL) was added and the reaction mixture extracted with ethyl acetate (3×150 mL). The combined organic layers were dried (magnesium sulfate), filtered, and evaporated to give a tan foam (2.65 g, 78%) which was pure by LC/MS (+APCI) m/z 326 (M+H+).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07129257B1 |
| 出典データセット | uspto-grants-2006_10 |
| ORD ID | ord-b0c0d8205a8f41f98ec32ad4ca9de451 |
| 出典メモ | uspto-grants-2006_10 |