33 b p 32 43 u00b0 0 07 mbar 1 h nmr 2 03 s 3h 3 03 s 3h 4 85 s 1h 6 44 s 1h 7 09 dd j 7 j 7 1h 7 11 d j 7 1h 7 22 m 1h 7 41 d j 7 1h 13 c nmr 145 9 s 143 9 s 141 8 s 128 7 d 128 4 d 124 6 d 123 7 d 120 1 d 84 9 d 51 8 q 14 1 q a solution of fecl 3 anhydrous 21 mg 0 125 mmol in buoac 2 ml was added dropwise during 5 minutes to a stirred solution of the 2 methyl 3 phenyl 2 propenylidene diacetate 3 1 g 12 5 mmol in buoac 8 ml at 123 u00b0 after 2 h at 123 u00b0 the reaction was stopped and worked up as above chromatography sio 2 cyclohex acoet 9 1 of the crude product allowed the isolation of the title acetate 62 yield identical spectra as previously described a solution of 2e 2 methyl 3 4 methylphenyl 2 propenal 100 0 g 0 62 mol in cyclohexane 300 0 g was added dropwise in 2 hours to a stirred solution of zinc chloride 3 1 g 22 mmol in acetic anhydride 188 4 g 1 85 mol at 80 u00b0 c the reaction mixture was stirred further at 80 u00b0 c for 18 hours and then cooled to 25 u00b0 c the mixture was washed twice with water 100 0 g and a 5 aqueous solution of sodium carbonate 100 0 g and concentrated under.