The preparation is in my scan of Biltz and Biltz. Also the 1909 (4th ed.) Gattermann, who states that the yield is at least equal to the weight of the
PCl3 (citing J Prakt 28, 382 (1883), https://doi.org/10.1002/prac.18830280131). The famous Fritz Ullmann recommends doing this diluted with premade POCl3 to avoid explosive reactions,
in Ber 34, 2172 (1901) (aka https://doi.org/10.1002/cber.190103402140) and says the yield is almost quantitative.
Needless to say, the reactions of P and P cpds. are not interchangeable with S.
[Edited on 16-9-2021 by S.C. Wack] |