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Azidotrimethylsilane → {[3-Azido-4-(2,4,5-trifluorophenyl)cyclohex-1-en-1-yl]oxy}(triisopropyl)silane
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Azidotrimethylsilane | HCID 78378 | — |
| 反応物 | Iodosylbenzene | HCID 92125 | — |
| 反応物 | Triisopropyl{[4-(2,4,5-trifluorophenyl)cyclohex-1-en-1-yl]oxy}silane | HCID 67065786 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | {[3-Azido-4-(2,4,5-trifluorophenyl)cyclohex-1-en-1-yl]oxy}(triisopropyl)silane | HCID 86616049 | — |
反応手順
In a three-neck flask, a stirred solution of triisopropyl{[4-(2,4,5-trifluorophenyl)cyclohex-1-en-1-yl]oxy}silane (26.06 g, 0.068 mol) in dichloromethane (260 mL) was cooled to −15° C. and treated with iodosobenzene (19.5 g, 0.089 mol) in four portions followed by azidotrimethylsilane (24 mL, 0.116 mol) while maintaining the temperature below −10° C. Stirring was continued for 1.5 h. The reaction mixture was allowed to warm to room temperature briefly, then cooled again back to −15° C. and filtered. The filtrate was evaporated under vacuum below 25° C. to give the title compound which was used directly in the next step.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07855206B2 |
| 出典データセット | uspto-grants-2010_12 |
| ORD ID | ord-54d91b88e8d345c4941710964aa324ab |
| 出典メモ | uspto-grants-2010_12 |