5-amino-2-methyl-2,3-dihydro-1H-isoindole-1,3-dione → 2-methyl-2,3-dihydro-1H-isoindol-5-amine
反応式
[NH2:1][C:2]1[CH:3]=[C:4]2[C:9](=O)[N:8]([CH3:11])[C:6](=O)[C:5]2=[CH:12][CH:13]=1.[H-].[Al+3].[Li+].[H-].[H-].[H-]>C1COCC1>[CH3:11][N:8]1[CH2:9][C:4]2[C:5](=[CH:12][CH:13]=[C:2]([NH2:1])[CH:3]=2)[CH2:6]1参加物
4
実験手順
2.643 g 4-Amino-N-methylphthalimide was suspended in 50 ml THF and added to 1.328 g lithium aluminum hydride in 50 ml THF at room temperature. The mixture was refluxed for 3 hrs, then stirred a further 3 days at room temperature. Excess LAH was destroyed by addition of water and the mixture filtered over celite. An aqueous phase was separated and extracted with CH2Cl2. The combined organic phases were dried and evaporated. The residue was stirred with HCl in MeOH and the evaporated to yield 1.6 g of the title compound as the hydrochlorid salt.
後処理
- temperatureThe mixture was refluxed for 3 hrs
- customExcess LAH was destroyed by addition of water
- filtrationthe mixture filtered over celite
- customAn aqueous phase was separated
- extractionextracted with CH2Cl2
- customThe combined organic phases were dried
- customevaporated
- stirringThe residue was stirred with HCl in MeOH
- customthe evaporated
出典と根拠
- ORDレコード
- ord-a2cdac2f4a86442e912f0760f5d995ae
- 出典データセット
- uspto-grants-2006_08
- 特許番号
- US07091345B2
反応ノート
読み込み中…