反应详情

温度

100 °C

3-Chloro-5-(1,3-dimethyl-2,4-dioxo-6-(2-(tritylthio)ethyl)-2,3,4,6-tetrahydro-1H-pyrrolo[3,4-d]pyrimidin-5-yl)benzonitrile (Intermediate GA) (146 mg, 0.237 mmol), 5-chlorofuran-2-carbaldehyde (34.0 mg, 0.260 mmol) and bismuth (III) triflate (31.0 mg, 0.047 mmol) were suspended in toluene (Volume: 2.5 ml). The reaction was then heated to 100° C. under microwave irradiation for 3 hr. The reaction mixture was suspended in MeOH (50 mL) and adsorbed onto silica. The residue was purified via ISCO SiO2 12 g Redisep Rf column eluting with 20% EtOAc/hexane. Fractions were combined and evaporated to afford a pale yellow gum. The gum was dissolved in Et2O (30 mL) and iso-hexane (30 mL) was added to afford a suspension. The solvent was evaporated to afford the title compound as a pale yellow solid.

1. customThe residue was purified via ISCO SiO2 12 g Redisep Rf column
2. washeluting with 20% EtOAc/hexane
3. customevaporated
4. customto afford a pale yellow gum
5. customto afford a suspension
6. customThe solvent was evaporated