反应详情

温度

85 °C

A 25-mL single-neck round-bottomed flask equipped with a magnetic stirrer and a reflux condenser was charged with 162a (197.6 mg, 1.3 mmol), tert-butanol (5.0 mL), triethylamine (262.6 mg, 2.6 mmol), and DPPA (550 mg, 2.0 mmol). The system was subjected to three cycles of vacuum/nitrogen flush and heated at 85° C. for 5 h. It was then cooled to room temperature and purified with Combiflash (A: 1% NH4HCO3/water, B: acetonitrile) to afford 162b (45 mg, 15.5%) as a yellow solid. MS-ESI: [M+H-56]+ 168.3

1. customA 25-mL single-neck round-bottomed flask equipped with a magnetic stirrer and a reflux condenser
2. customflush
3. temperatureIt was then cooled to room temperature
4. custompurified with Combiflash (A: 1% NH4HCO3/water, B