関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | 3-Nitrobenzenesulfonyl chloride | HCID 8476 | — |
| 反応物 | N-Boc-2-(4-aminophenyl)ethanol | HCID 11413715 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | 4-(Tert-butoxycarbonylamino)phenethyl 3-nitro-benzenesulfonate | HCID 54535442 | 47% |
反応手順
2-[4-(tert-butoxycarbonylamino)phenyl]-1-ethanol dissolved in dichloromethane. The reaction mixture was cooled to −25° C. and 9.34 g (42 mmole) 3-nitrobenzenesulfonyl chloride was added in portions. The reaction mixture was poured on to icewater, the phases were separated and the organic phase was dried (sodium sulfate), filtered and the solvent was evaporated in vacuo. The residue was purified by chromatography on silica gel using dichloromethane as eluent to give 8.3 g (yield 47%) 4-(tert-butoxycarbonylamino)-phenethyl 3-nitro-benzenesulfonate as yellow crystals.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US06288096B1 |
|---|
| 出典データセット | uspto-grants-2001_09 |
|---|
| ORD ID | ord-79a2174653aa4d7689200bc2493fb569 |
|---|
| 出典メモ | uspto-grants-2001_09 |
|---|
