反应详情

To a slurry of 1.1 g of (+/-)-α-(chloromethyl)-4'-[(difluoromethyl)thio][1,1'-biphenyl]-4-methanamine hydrochloride in 13 mL of ethyl acetate was added 0.60 g of 2.6-difluorobenzoyl chloride. 0.60 g of sodium bicarbonate, and 3 mL of water. After 15 min, ethyl acetate was added and the organic phase was washed with aqueous NaCl, dried (MgSO4), filtered, and concentrated to dryness. The residue was triturated with toluene/hexanes, filtered, washed with hexanes, and suction-dried to afford 1.22 g of product, m.p. 148-150° C. 1H-NMR (CDCl3): δ4.0 (dq, 2H), 5.6 (m, 1H), 6.75 (br d, 1H), 6.85 (t, 1H, J=60 Hz), 7.0 (t, 2H), 7.4 (m, 1H), 7.5 (d, 2H), 7.6 (m, 6H).

1. washthe organic phase was washed with aqueous NaCl
2. dry with materialdried (MgSO4)
3. filtrationfiltered
4. concentrationconcentrated to dryness
5. customThe residue was triturated with toluene/hexanes
6. filtrationfiltered
7. washwashed with hexanes
8. customsuction-dried