反应详情

温度

100 °C

Triethylamine (765 μl), tert-butylalcohol (10 ml), and DPPA (1.18 ml) were added to a 1,4-dioxane (20 ml) solution containing 2-methyl-1,3-benzoxazol-6-carboxylic acid (885 mg), followed by stirring at 100° C. for 1 hour and 30 minutes. The solvent was distilled away under reduced pressure, and a saturated aqueous sodium hydrogen carbonate solution and ethyl acetate were added. The organic layer was collected, washed with saturated saline, and dried over anhydrous sodium sulfate, and then the solvent was distilled away under reduced pressure. The obtained residue was purified by silica gel column chromatography, and a white solid of tert-butyl(2-methyl-1,3-benzoxazol-6-yl)carbamate (1.00 g) was thus obtained.

1. distillationThe solvent was distilled away under reduced pressure
2. additiona saturated aqueous sodium hydrogen carbonate solution and ethyl acetate were added
3. customThe organic layer was collected
4. washwashed with saturated saline
5. dry with materialdried over anhydrous sodium sulfate
6. distillationthe solvent was distilled away under reduced pressure
7. customThe obtained residue was purified by silica gel column chromatography