A Convenient Preparation of Isothiocyanates

✍ Scribed by Dr. R. Gottfried

• Publisher: John Wiley and Sons
• Year: 1966
• Tongue: English
• Weight: 249 KB
• Volume: 5
• Category: Article
• ISSN: 0044-8249
• DOI: 10.1002/anie.196609632

✦ Synopsis

mixture with heptane, from which it is crystallized a t -80 "C.

The yield was 27 % calculated on the total amount of starting material, and 54 "/, on the amount consumed. CzH5Cp2ZrCI is a crystalline, intensely yellow, diamagnetic compound [xg = -(0.44 & 0.04) x 10-6 E.M.U./g], which is decomposed by light, air, or water. It is stable under nitrogen a t 0 "C. C2H5Cp2ZrCI (1.4 mmole) was treated with AI(C2Hs)j (14.7 mmole) at 2OoC and atmospheric pressure. The chloride dissolved rapidly and a yellow-red color developed. After a short time, gas evolution began and the color deepened. Only ethane was evolved, whereas in the corresponding reaction of the titanium compound ethane and ethylene were formed. After 19 min, 1 mole of C2H6 had been liberated per gramatom of zirconium. The time-yield curve for the evolution of the first mole of C2H6 indicates a reaction of the second order with respect to zirconium. Two moles of ethane are evolved per gram atom of zirconium within 24 hours.

When gas evolution had ceased the mixture had a susceptibility xg of -(0.69 :!. 0.02) x 10-6, i.e. the compound formed by loss of ethane is diamagnetic.