What Are Synthesis Methods of Tungsten Tetrachloride?

1. In a drying oven filled with inert gas, put 5g of tungsten hexachloride and a stirring rod made of polytetrafluoroethylene together, and put it into 6 at the 4th place of the device as shown in the “tungsten tetrachloride synthesis device”, Subsequently, the branch pipe 4 is melt-sealed. Cool 6 places with dry ice, and simultaneously open the cock made of polytetrafluoroethylene to suck air from 2 places. Using the vacuum distillation method, introduce the refined and dehydrated tetrachlorethylene from the outside to 6 places to reach 30mL. After returning to normal temperature, vacuumize and immerse 6 places in a transparent oil bath, irradiate with a 500W bulb, and react at 150°C for 3 days. At this time, for safety reasons, the reaction device may be surrounded by a protective screen. Cool down after the reaction, then turn the apparatus upside down, and filter the resulting precipitate through a glass filter 3 . If one place is heated again, the unreacted tungsten hexachloride attached to the precipitate is extracted due to the reflux of the organic solvent, and the heating is stopped after the extract becomes colorless. Next, air was drawn from two places, and the cock made of polytetrafluoroethylene was opened, and the organic solvent was completely expelled by distillation under reduced pressure. In a dry box filled with inert gas, cut off at 6 points, and take out the product on the glass filter. The product contains impurities such as tungsten pentachloride produced by side reactions, so it is placed in a hard glass tube. If it is heated in a carbon dioxide gas stream, the most volatile tungsten pentachloride in tungsten chloride It will be sublimated first, and when the temperature is raised again, tungsten hexachloride and tungsten dichloride will also volatilize, and only the target product tungsten tetrachloride will not sublime and finally remain. The yield is 95%.
2. Add 20-25g of tungsten hexachloride and the calculated amount of aluminum foil into a borosilicate glass tube with a diameter of 30mm (the excess of tungsten hexachloride is 1-2g). Then, the reaction tube was evacuated and sealed. The reaction tube was kept at 475° C., and the end containing tungsten hexachloride was kept at 225° C. After about 48 hours, the reaction was completed. During the reaction, the product tungsten tetrachloride can diffuse to the colder end of the tube and condense as a coarse crystalline deposit. In order to remove excess tungsten hexachloride and the generated aluminum chloride, the end of the tube containing the crystalline powder was heated at 225°C, and the other end was kept at room temperature. Then, open the reaction tube in the dry box, and take out the tungsten tetrachloride.
3. Computing chemical data
   1. Hydrophobic parameter calculation reference value (XlogP): None
   2. Number of hydrogen bond donors: 0
   3. Number of hydrogen bond acceptors: 0
   4. Number of rotatable chemical bonds: 0
   5. Number of tautomers: none
   6. Polar surface area of topological molecules: 0
   7. Number of heavy atoms: 5
   8. Surface charge: 0
   9. Complexity: 19.1
   10. Number of isotope atoms: 0
   11. Determine the number of atomic stereocenters: 0
   12. Uncertain number of atomic stereocenters: 0
   13. Determine the number of stereocenters of chemical bonds: 0
   14. Uncertain number of chemical bond stereocenters: 0
   15. Number of covalent bond units: 1
       
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