化工社化工社 化学情報印刷レポート · 研究参考用
Diphenylsilane → 1,1-Dimethylethyl 1-(4-chlorophenyl)-2-cyclopropyl-2,7-diazaspiro[3.5]nonane-7-carboxylate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Diphenylsilane | HCID 69888 | — |
| 反応物 | 1,1-Dimethylethyl 1-oxo-3-(4-chlorophenyl)-2-cyclopropyl-2,7-diazaspiro[3.5]nonane-7-carboxylate | HCID 24954507 | — |
| 触媒 | Carbonylhydridotris(triphenylphosphine)rhodium(I) | HCID 10941995 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | 1,1-Dimethylethyl 1-(4-chlorophenyl)-2-cyclopropyl-2,7-diazaspiro[3.5]nonane-7-carboxylate | HCID 57986042 | 95.5% |
反応手順
Under a nitrogen atmosphere, treat 1,1-dimethylethyl 1-oxo-3-(4-chlorophenyl)-2-cyclopropyl-2,7-diazaspiro[3.5]nonane-7-carboxylate (9) (0.76 g) in anhydrous THF (2 mL) with RhH(CO)(PPH3)3 (18 mg) and then, diphenylsilane (9.1 mL). The resulting mixture was shaken at room temperature for 2 h. Place the reaction mixture on silica gel plates (12, 1000 u) and elute with hexane/EtOAc 85/15 to give a colorless residue (0.700 g). Place this material on silica gel plates (12, 1000 u) and elute with hexane/EtOAc 85/15 to give the title compound (10) as a colorless foam (0.58 g)
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07638526B2 |
| 出典データセット | uspto-grants-2009_12 |
| ORD ID | ord-50fd09f961b948ee9b00b4150ec544bb |
| 出典メモ | uspto-grants-2009_12 |