Boron trifluoride etherate → HCID 10450370, compound

Participants

Reaction Conditions

Reaction Steps

The mixture of 0.9 g (3.3 m mol) of 4-methylsulfonylphenyl-actophenone prepared in Example 97 and 0.5 g (3.3m mol) of phenylhydrazine hydrochloride were heated at 130° C. for 0.5 h. After cooling, 20 ml of acetic acid and 0.2 g of BF3.Et2O was added and heated to reflux for 1 h. Acetic acid was removed in vacuo, the resulting residue was suspended in water, filtered, dried and purified by column chromatography using petroleum ether/ethyl acetate 3:1 as elutant, 0.45 g of the title compound was obtained as white crystal, yield, 39.5%, m.p. 239-241° C. The data of Nuclear Magnetic Resonance shown that: 1HNMR (300 MHz, DMSO)δ: 3.24 (s, 3H, SO2CH3), 7.05-7.90 (m, 13H, Ar—H), 11.77 (s, 1H, N—H); Anal. Calcd for: C21H17NO2S: C 72.60, H 4.93, N 4.03; Found: C 72.35, H 5.03, N 4.25.

Provenance & Evidence