Diethyl Oxalate → HCID 53863676、化合物
反応式
[CH3:1][C:2]1[CH:3]=[CH:4][C:5]([NH2:15])=[C:6]2[C:10]=1[CH:9]([CH2:11][CH2:12][CH3:13])[CH2:8][C:7]2=[O:14].[CH2:16]([O:18][C:19](=[O:25])[C:20](OCC)=[O:21])[CH3:17]>>[CH2:16]([O:18][C:19](=[O:25])[C:20]([NH:15][C:5]1[CH:4]=[CH:3][C:2]([CH3:1])=[C:10]2[C:6]=1[C:7](=[O:14])[CH2:8][CH:9]2[CH2:11][CH2:12][CH3:13])=[O:21])[CH3:17]参加物
3
実験手順
A solution of 7.2 g of 7-methyl-3-oxo-1-propyl-4-indanylamine in 34 ml oxalic acid diethyl ester is boiled under reflux for 2 hours and then cooled to room temperature. The reaction mixture is then heated at 90°-100° at 11 mm Hg to remove the excess oxalic acid diethyl ester. The residue is chromatographed on 200 g silica gel to afford the pure title compound which is recrystallised from ether. M.pt. 84°-86°.
後処理
- temperatureunder reflux for 2 hours
- temperatureThe reaction mixture is then heated at 90°-100° at 11 mm Hg
- customto remove the excess oxalic acid diethyl ester
- customThe residue is chromatographed on 200 g silica gel