反应详情

温度

0 °C

Triphosgene (95 mg) was added to a solution of methyl 2-aminobenzoate (120 mg) and triethylamine (0.17 mL) in toluene (5 mL), and the mixture was stirred at 0° C. for 30 min. To the reaction mixture were added tert-butyl (6SR,7RS)-7-(aminomethyl)-6-(3,4-dichlorophenyl)-1,4-oxazepane-4-carboxylate (300 mg) and triethylamine (0.17 mL), and the mixture was stirred at room temperature for 1 hr. Water was added to the reaction mixture, and the mixture was extracted with ethyl acetate. The extract was washed with brine, and dried over anhydrous sodium sulfate. The solvent was evaporated under reduced pressure. The residue was purified by silica gel column chromatography to give the title compound (190 mg).

1. stirringthe mixture was stirred at room temperature for 1 hr
2. extractionthe mixture was extracted with ethyl acetate
3. washThe extract was washed with brine
4. dry with materialdried over anhydrous sodium sulfate
5. customThe solvent was evaporated under reduced pressure
6. customThe residue was purified by silica gel column chromatography