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Triphenylphosphine → t-Butyl 4-(4-trifluoromethylsulfanyl-phenoxy)piperidine-1-carboxylate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Triphenylphosphine | HCID 11776 | — |
| 反応物 | ethyl N-ethoxycarbonyliminocarbamate | HCID 220568 | — |
| 反応物 | Tert-butyl 4-hydroxypiperidine-1-carboxylate | HCID 643502 | — |
| 反応物 | 4-(Trifluoromethylsulfanyl)phenol | HCID 3815158 | — |
| 溶媒 | Water | HCID 962 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | t-Butyl 4-(4-trifluoromethylsulfanyl-phenoxy)piperidine-1-carboxylate | HCID 22031376 | 79.1% |
反応手順
A solution of 2 g 4-trifluoromethylsulfanyl-phenol, 2.07 g t-butyl 4-hydroxy-1-piperidinecarboxylate, 3.2 g triphenyl phosphine and 5.4 g diethyl azodicarboxylate (40% toluene solution) in anhydrous tetrahydrofuran (40 mL) was heated for 24 hours under reflux in a stream of nitrogen. Water was added thereto, and the reaction solution was extracted with ethyl acetate, dried over sodium sulfate, and purified by NH silica gel chromatography (hexane/ethyl acetate) to give 3.07 g of the title compound.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07074801B1 |
| 出典データセット | uspto-grants-2006_07 |
| ORD ID | ord-974ff422334b47ba88b6df9ed7b633cf |
| 出典メモ | uspto-grants-2006_07 |