Phthalic Anhydride → 2-(Dimethylamino)isoindoline-1,3-dione
反応式
[C:1]1(=O)[O:6][C:4](=[O:5])[C:3]2=[CH:7][CH:8]=[CH:9][CH:10]=[C:2]12.Cl.Cl.[CH3:14][N:15]([CH3:17])[NH2:16].C(N(CC)C1C=CC=CC=1)C>C1(C)C=CC=CC=1>[CH3:14][N:15]([CH3:17])[N:16]1[C:4](=[O:5])[C:3]2[C:2](=[CH:10][CH:9]=[CH:8][CH:7]=2)[C:1]1=[O:6]参加物
5
実験手順
To the suspension of phthalic anhydride (62.5 mmol) in toluene (500 ml), N,N-dimethyl hydrazine dihydrochloride (50 mmol) and diethyl-phenyl-amine (90 mmol) were added. The reaction mixture was refluxed for 18 hours while removing the formed water via a Dean-Stark trap. Then, toluene was evaporated under reduced pressure and the resulting crude was purified on silica gel chromatography with (1:5) EtOAc:dichloromethane, to give the desired product in 85% yield.
後処理
- additionwere added
- temperatureThe reaction mixture was refluxed for 18 hours
- customwhile removing the formed water via a Dean-Stark trap
- customThen, toluene was evaporated under reduced pressure
- customthe resulting crude was purified on silica gel chromatography with (1:5) EtOAc
出典と根拠
- ORDレコード
- ord-9556816542c64a74867182946ad62c50
- 出典データセット
- uspto-grants-2013_09
- 特許番号
- US08541428B2
反応ノート
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