反应详情

温度

80 °C

A sol. of 2,6-dichloro-p-cresol (0.55 mmol; 97 mg) in toluene (4.8 mL) was treated with compound E9 (0.37 mmol; 250 mg) followed by azodicarboxylic dipiperidide (0.73 mmol; 184 mg) and PBu3 (1.28 mmol; 0.27 mL). The reaction mixture was stirred at 80° C. After 1 h, the reaction mixture was allowed to cool to rt, diluted with Et2O (50 mL), filtrated, and the filtrate was washed with NaOH 1M (50 mL) and brine (50 mL). The org. extract was dried over MgSO4, filtered, and the solvents were removed under reduced pressure. Purification of the residue by FC (EtOAc/heptane 30:70) yielded the title compound (0.23 g, 76%). LC-MS: tR=1.25 min; ES+: 843.29.

1. temperatureto cool to rt
2. filtrationfiltrated
3. washthe filtrate was washed with NaOH 1M (50 mL) and brine (50 mL)
4. extractionextract
5. dry with materialwas dried over MgSO4
6. filtrationfiltered
7. customthe solvents were removed under reduced pressure
8. customPurification of the residue by FC (EtOAc/heptane 30:70)