反应详情

温度

110 °C

A 250-mL round-bottomed flask equipped with a magnetic stirrer was charged with 287c (10.4 g, 1.0 eq., 41.9 mmol), tert-butyl 2-chloroethylcarbamate (37.7 g, 5.0 eq., 210.0 mmol), Na2CO3 (22.3 g, 5.0 eq., 210.0 mmol), and DMF (100 mL). The reaction mixture was stirred at 110° C. overnight. After cooling to room temperature, the resulting mixture was poured into water (200 mL) and extracted with ethyl acetate (3×100 mL). The combined organic layer was concentrated under reduced pressure. The resulting residue was purified by silica-gel column chromatography eluting with ethyl acetate to afford 287d (10.8 g, 66%) as yellow oil. MS-ESI: [M+H]+ 392.0

1. customA 250-mL round-bottomed flask equipped with a magnetic stirrer
2. temperatureAfter cooling to room temperature
3. extractionextracted with ethyl acetate (3×100 mL)
4. concentrationThe combined organic layer was concentrated under reduced pressure
5. customThe resulting residue was purified by silica-gel column chromatography
6. washeluting with ethyl acetate