反应详情

Three grams (0.01 mole) of 4-(3-methylphenyl-hydrazono)-2-phenyl-oxazoline-5-one (R1 =3--CH3, R2 =R3 =H in the formula II) was suspended in 93 ml of methanol. To the resulting suspension, 66.2 ml of 29% solution of ammonium hydroxide (0.549 mole) was added and refluxed for 5 minutes. Methanol and ammonia were then distilled off under a reduced pressure, and the resulting crystals were filtered out and washed with water. The crystals were recrystallized from a mixed solvent of 5.8 ml of methanol and 4.5 ml of water to obtain 1.8 g of almost colorless crystal, m.p. 142°-143° C., with a yield of 63%. I.R. (KBr, cm-1, refer to FIG. 2); 3500-3240 (broad and strong), 1700, 1670, 1610, 1458, 1400, 1302, 789 and 700.

1. temperaturerefluxed for 5 minutes
2. distillationMethanol and ammonia were then distilled off under a reduced pressure
3. filtrationthe resulting crystals were filtered out
4. washwashed with water
5. customThe crystals were recrystallized from a mixed solvent of 5.8 ml of methanol and 4.5 ml of water
6. customto obtain 1.8 g of almost colorless crystal, m.p. 142°-143° C.