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Triphenylphosphine → N-cyclopropyl-N-[1-(2-naphthyl)ethyl]-2-nitrobenzenesulfonamide
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Triphenylphosphine | HCID 11776 | — |
| 反応物 | Diisopropyl diazene-1,2-dicarboxylate | HCID 75555 | — |
| 反応物 | alpha-Methylnaphthalene-2-methanol | HCID 98243 | — |
| 反応物 | N-cyclopropyl-2-nitrobenzenesulfonamide | HCID 796630 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | N-cyclopropyl-N-[1-(2-naphthyl)ethyl]-2-nitrobenzenesulfonamide | HCID 86707860 | 63% |
反応手順
To a solution of 1-(2-naphthyl)ethanol (344 mg), N-cyclopropyl-2-nitrobenzenesulfonamide (581 mg) and triphenylphosphine (787 mg) in tetrahydrofuran (10 mL) was added dropwise diisopropyl azodicarboxylate (590 μL) under ice-cooling, and the mixture was stirred at room temperature for 3 hours. The reaction solution was concentrated, and the resulting residue was purified by silica gel column chromatography (eluent: n-hexane/ethyl acetate=4/1→1/1), and then triturated with diethyl ether-n-hexane (1:1) to give N-cyclopropyl-N-[1-(2-naphthyl)ethyl]-2-nitrobenzenesulfonamide j[REx(1-1)] (499 mg) as a colorless powder.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US09278944B2 |
| 出典データセット | uspto-grants-2016_03 |
| ORD ID | ord-ee73abe846394dbf8b14aa530845d304 |
| 出典メモ | uspto-grants-2016_03 |