関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Tetrahydrofuran | HCID 8028 | — |
| 反応物 | Triphenylphosphine | HCID 11776 | — |
| 反応物 | Carbonic acid, bis(1,1-dimethylethyl) ester | HCID 10219638 | — |
| 反応物 | (1R,2S)-1-azido-1-(3,4,5-trifluorophenyl)propan-2-ol | HCID 86612610 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | tert-butyl [(1R,2S)-2-hydroxy-1-(3,4,5-trifluorophenyl)propyl]carbamate | HCID 68717988 | 86.3% |
反応手順
In nitrogen atmosphere, triphenylphosphine (5.85 g) was added to a THF solution (75 mL) of (1R,2S)-1-azido-1-(3,4,5-trifluorophenyl)propan-2-ol (5.16 g). This reaction solution was stirred at room temperature for 10 min, then water (5 mL) was added the reaction solution. This mixture was stirred at 60° C. for 3.5 hr. The reaction solution was cooled to room temperature, and then di-tert-butylcarbonate (5.35 g) was added to the reaction solution. The resulting reaction solution was stirred at room temperature for 45 min and then concentrated under reduced pressure. The obtained residue was purified by silica gel column chromatography (toluene:ethyl acetate=9:1) to give 5.88 g of the title compound. The physical property values of this compound were as follows:
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07737141B2 |
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| 出典データセット | uspto-grants-2010_06 |
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| ORD ID | ord-9b929db65e1f4d39ba38def4d69f12d7 |
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| 出典メモ | uspto-grants-2010_06 |
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