反应详情

温度

90 °C

In a screw-capped vial (8 mL) was placed dry degassed triethylamine (4.0 mL) and a magnetic stirrer under argon. Compound 495 (100 mg, 0.21 mmol), Pd2(dba)3 (3.8 mg), triphenyl phosphine (5.4 mg, 0.02 mmol), CuI (1 mg) and ethynyl-trimethyl-silane (29 μL, 0.21 mmol) were added to the vial and the reaction mixture was heated under vigorously stirring at 90° C. for 20 h. The cooled reaction mixture was filtered through Decalite and concentrated in vacuo. The crude product was purified by continuous gradient flash chromatography using EtOAc/petroleum ether (40-60) (v:v=0:100 to 10:90) as the eluent to afford the title compound as foam.

1. customIn a screw-capped vial (8 mL) was placed dry
2. customdegassed triethylamine (4.0 mL) and a magnetic stirrer under argon
3. temperaturewas heated
4. customThe cooled reaction mixture
5. filtrationwas filtered through Decalite
6. concentrationconcentrated in vacuo
7. customThe crude product was purified by continuous gradient flash chromatography