Berlin blue in water boiling for several hours at 3 atm;
参考文献
Gmelin Handbook: K: MVol.4, 5.1, page 894 - 901
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反应条件
CaO in not given byproducts: CaSO4; formation of CaSO4, KHS and K2S2O3 from mixt. of K2SO4 (soln.), S and CaO; addn. of CaCN2 to hot soln. leads to formation of CS(NH2)2 which further reacts with KHS to yield KCNS.;
disulfur dichloride; iron(III) chloride in neat (no solvent) addn. of a mixt. of 140 g PCl3 and 1.7 g S2Cl2 drop by drop to a hot mixt. of 160 g PSCl3, 2 g anhydrous FeCl3 and 38 g S on stirring and refluxing (4.5 h); refluxing for 1 h, distg. off PSCl3;;
aluminium trichloride in neat (no solvent) heating PCl3 with S and AlCl3 (catalyst) under exclusion of H2O; react. with the intermediate AlCl3*PCl3; addn. of AlCl3 in small portions to the boiling mixt. of PCl3 and S, react. on boiling completed after 10 min;; extraction of the cold crude product with H2O and separation with a separatory funnel; drying over CaCl2 and distn. at 125-126 °C at ambient pressure;;
