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Tributylphenyltin → HCID 178523764、化合物
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Tributylphenyltin | HCID 607632 | — |
| 反応物 | HCID 178523770 | HCID 178523770 | — |
| 触媒 | HCID 178418476 | HCID 178418476 | — |
| 溶媒 | 1,4-Dioxane | HCID 31275 | — |
| 生成物 | HCID 178523764 | HCID 178523764 | 77.4% |
反応手順
Under argon atmosphere, a mixture comprising 1.0 g trans-4-(benzyloxycarbonylamino)cyclohexanecarbonyl chloride, 1.92 g of tributylphenyltin, 61 mg of dichlorobis(triphenylphosphine)palladium and 10 mL of dioxane was stirred at 110° C. for 12 hours. After cooling, the reaction mixture was concentrated by a centrifugal concentrator, and then, the residue was dissolved in tetrahydrofuran and evaporated to dryness with 5 g of silica gel. The resulting residue was purified by silica gel flash chromatography (solvent: ethyl acetate-hexane (1:2) to (1:1) to obtain 883 mg of N-benzyloxycarbonyl-trans-4-benzoylcylohexylamine.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06849622B2 |
| 出典データセット | uspto-grants-2005_02 |
| ORD ID | ord-7c06d5bd97d64f32bf7b3094cb12d110 |
| 出典メモ | uspto-grants-2005_02 |