関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Azidotrimethylsilane | HCID 78378 | — |
| 反応物 | Benzene, 1-bromo-4-ethynyl- | HCID 136603 | — |
| 反応物 | Sodium Ascorbate | HCID 23667548 | — |
| 溶媒 | Water | HCID 962 | — |
| 溶媒 | tert-Butanol | HCID 6386 | — |
| 生成物 | HCID 178419355 | HCID 178419355 | — |
反応手順
1-Bromo-4-ethynylbenzene (650 mg, 3.59 mmol) and trimethylsilyl azide (3.57 mL, 26.9 mmol) were combined in t-BuOH (5.0 mL) and water (3.0 mL) CuSO4.5H2O (90 mg, 0.36 mmol) in water (1.0 mL) and sodium ascorbate (285 mg, 1.44 mmol) in water (1.0 mL) were added, and the sealed reaction mixture was stirred at 100° C. for 48 h. The mixture was diluted with water and extracted with EtOAc (3×). The combined organic layers were washed with brine, dried (MgSO4), filtered, and evaporated. Flash chromatography (dry load, 0-50% EtOAc/hexanes) afforded the title compound as a colorless solid.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08367706B2 |
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| 出典データセット | uspto-grants-2013_02 |
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| ORD ID | ord-e1d2c4c42db4498d8be0729f57f379c5 |
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| 出典メモ | uspto-grants-2013_02 |
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