NiCl2 + Concentrated HCl produces a powerful chlorinating reagent call the Lucas Reagent.
If you reduce the NiCl2 with Zn dust you get an activated Ni Catalyst.
SYNTHESIS OF HALO-EPHEDRINE
CHLOROEPHEDRINE is best synthesized with (ZnCl2 + con.HCl) or (CaCl2 + con.HCl) + EPHEDRINE ==>> C6H5-(CHCl)-CH(NHCH3)-CH3
PROCEDURE 1 : Arrange a 250 ml round-bottom with a reflux condenser, the top is connected to a device or absorbing excess HCl. Place 68 grams (0.5 mole) of anhydrous zinc chloride (ZnCl2), 50 mls of concentrated HCl, and 50.43 grams (0.25 mole) of EPHEDRINE HCl. Reflux the mixture gently for 2 hours.
PROCEDURE 2 : Arrange a 1000 ml round-bottom with a reflux condenser, the top is connected to a device or absorbing excess HCl. Place 80 grams of anhydrous calcium chloride (CaCl2), 250 mls of concentrated HCl, and 100.9 (101) grams (0.5 mole) of EPHEDRINE HCl. Heat the mixture gently for 10 hours on a boiling water bath.
In both PROCEDURE 1 and PROCEDURE 2, basify the reaction mixture with 20 % sodium hydroxide solution.
The libertated freebase CHLOROEPHEDRINE which seperates is solvent extracted with two, 75 - 100 ml ether (or toluene) portions and the ether/CHLOROEPHEDRINE solution is washed with 2 x 50 mls of distilled water.
The solvent is removed to give CHLOROEPHEDRINE FREEBASE in 70 - 76% yield.
EPHEDRINE FREEBASE in ether with THIONYL CHLORIDE (SOCl2), DOES NOT WORK WELL, AS EPHEDRINE HCl IS PRECIPITATED OUT.
IT DOES WORK WELL WITH C6H5-(CHOH)-CH(NO2)-CH3, GIVING 95 - 97% YIELD.