反应详情

To a solution of α-(α,α,α-trifluoro-m-tolyl)-4-morpholineacetonitrile in 100 ml. of tetrahydrofuran is added 1.0 ml. of 30% KOH-ethanol solution. To the mixture is added 2.56 g. of crotononitrile and the mixture is stirred at room temperature for 18 hrs. The mixture is concentrated to dryness under vacuum and the residue is dissolved in chloroform. The solution is passed through a column of hydrous magnesium silicate. The eluent is concentrated to an oil (17.3 g) which is crystallized from hexane and recrystallized from CHCL3 -hexane to give 3-methyl-2-morpholino-2-(α,α,α-trifluoro-m-tolyl)glutaronitrile as crystals, m.p. 115°-118° C.

1. additionTo the mixture is added 2.56 g
2. concentrationThe mixture is concentrated to dryness under vacuum
3. dissolutionthe residue is dissolved in chloroform
4. concentrationThe eluent is concentrated to an oil (17.3 g) which
5. customis crystallized from hexane
6. customrecrystallized from CHCL3 -hexane