sodium T=140°C;

in not given

in not given

1: not given 2: NaOH / sodium hydroxide View Scheme

HCl in tetrahydrofuran N2 or Ar atmosphere; addn. of THF to ZrCl4 (-78°C), warming (room temp.), stirring (1 h), addn. of soln. of org. compd. in THF, stirring (1 h, room temp.), cooling (0°C), bubbling of HCl into soln.; partial evapn., addn. of Et2O, centrifugation, drying (vac.), sublimation (200-220°C, 0.03 mmHg); elem. anal.;

in tetrahydrofuran heating (60°C, 72 h), solvent removal (red. press.), residue extd. (toluene), volatiles removal (red. pressure), residue extd. (light petroleum, b.p. 40-60°C); chromy. (alumina), elution (light petroleum); collection of bright yellow band, concn. (red. pressure), cooling (-80°C, 24 h) on crystn., drying (vac.); elem. anal.;