Gamma-Butyrolactone → 1-(2H-1,3-Benzodioxol-5-yl)pyrrolidin-2-one
反応式
[CH2:1]1[O:10][C:9]2[CH:8]=[CH:7][C:5]([NH2:6])=[CH:4][C:3]=2[O:2]1.[C:11]1(=O)[O:15][CH2:14][CH2:13][CH2:12]1>>[O:10]1[C:9]2[CH:8]=[CH:7][C:5]([N:6]3[CH2:11][CH2:12][CH2:13][C:14]3=[O:15])=[CH:4][C:3]=2[O:2][CH2:1]1参加物
3
実験手順
A mixture of 3,4-(methylenedioxy)aniline (200 g, 1.46 mole) and γ-butyrolactone (225 ml) was heated (in a dry nitrogen atmosphere) with stirring in a 200° oil bath for 2 days. Product was isolated from the reaction mixture by distillation under reduced pressure (b.p. 156°, 33 μ). Product was filtered over Silica Gel 60 (Trade Name) eluting with ethylacetate. The eluant was concentrated and the crystalline product was collected and washed with ether and petroleum ether affording 1-(1,3-benzodioxol-5-yl)-2-pyrrolidinone (153.4 g; 51%), m.p. 89°-91° which was one spot on tlc analysis.
後処理
- temperaturewas heated (in a dry nitrogen atmosphere)
- customProduct was isolated from the reaction mixture by distillation under reduced pressure (b.p. 156°, 33 μ)