反应详情

温度

-25 °C

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.

1. additionThe reaction mixture was poured on to icewater
2. customthe phases were separated
3. dry with materialthe organic phase was dried (sodium sulfate)
4. filtrationfiltered
5. customthe solvent was evaporated in vacuo
6. customThe residue was purified by chromatography on silica gel