反应详情

A solution of 42.3 g (0.377 mol) of 75% pure 1-amino-1H-1,2,4-triazole, 40.0 mL (0.372 mol) of 4-fluorobenzaldehyde and 2.0 g of p-toluenesulfonic acid in 600 mL of tetrahydrofuran was stirred at room temperature for 21/2 days. The reaction mixture was diluted with ethyl acetate, washed with saturated aqueous Na2CO3, water and brine and dried (MgSO4). Removal of solvent gave a white solid which was recrystallized from n-butylchloride to afford 48.3 g (67%) of desired product as white needles; mp 118°-120° C. Concentration of the filtrate and recrystallization of the residue afforded 12.8 g (18%) more of product; mp 118°-120° C.

1. washwashed with saturated aqueous Na2CO3, water and brine
2. dry with materialdried (MgSO4)
3. customRemoval of solvent
4. customgave a white solid which
5. customwas recrystallized from n-butylchloride