反应详情

To a suspension of 3,7-bis-benzyloxynaphthalene-2-carboxylic acid (0.768 g, 2 mmol) in anhydrous t-BuOH (8 mL) and anhydrous toluene (8 mL) is added triethylamine (0.303 g, 3 mmol). To the resulting solution is added DPPA (0.715 g, 2.6 mmol) and the mixture is stirred at room temperature for 5 min, then stirred at 100° C. for 18 h. The mixture is allowed to cool to room temperature and then poured into water. The mixture is extracted into EtOAc and the organic phase is washed with saturated NaCl. The solvent is removed-under reduced pressure and the resulting residue is purified by flash chromatography, eluting with DCM to afford (3,7-bis-benzyloxynaphthalene-2-yl)-carbamic acid tert-butyl ester as a white solid: mp=179-182° C.

1. stirringstirred at 100° C. for 18 h
2. temperatureto cool to room temperature
3. extractionThe mixture is extracted into EtOAc
4. washthe organic phase is washed with saturated NaCl
5. customthe resulting residue is purified by flash chromatography
6. washeluting with DCM