Scheme 2: Synthesis of phosphorothioate from two components and 3A X-ray single crystal diffraction.
Phenylacetylene (1.2 mmol, 122.6 mg), 2d (1.0 mmol, 234.3 mg) and toluene (5 mL) were added to the tube and sealed. Then BF3·OEt2 (1.0 mmol, 265 μL) was injected into the sealed tube by micro-syringe. After reacting at 90 °C for 5 min, the reaction solution was warmed to room temperature, and the mixture was left to stand overnight at 0 °C. A large amount of colorless transparent solid precipitated. A small portion of the solid is taken out for X-ray single crystal diffraction analysis.
