Hydrochloric Acid → 2-(1,3-Isoindolinedion-2-yl)-5-(3-carboxy-3,3-dimethylpropionyl)indane
반응식
[Cl-].[Al+3].[Cl-].[Cl-].C[CH:6]1[CH:11]([CH3:12])[C:10](=[O:13])[O:9][C:7]1=[O:8].[C:14]1(=[O:33])[C:22]2[C:17](=[CH:18][CH:19]=[CH:20][CH:21]=2)[C:16](=[O:23])[N:15]1[CH:24]1[CH2:32][C:31]2[C:26](=[CH:27][CH:28]=[CH:29][CH:30]=2)[CH2:25]1.Cl.[C:35](=S)=S>>[C:14]1(=[O:33])[C:22]2[C:17](=[CH:18][CH:19]=[CH:20][CH:21]=2)[C:16](=[O:23])[N:15]1[CH:24]1[CH2:25][C:26]2[C:31](=[CH:30][CH:29]=[C:28]([C:7](=[O:8])[CH2:6][C:11]([C:10]([OH:9])=[O:13])([CH3:12])[CH3:35])[CH:27]=2)[CH2:32]1참가 물질
6
실험 절차
in 30 ml of carbon disulfide was suspended 1.60 g of anhydrous aluminum chloride, and to the suspension were added under ice cooling 580 mg of dimethyl succinic anhydride and then 790 mg of 2-(1,3-isoindolinedion-2-yl)indane. The mixture was stirred at 0° C. to room temperature for 3 hours and then refluxed under heating for 4 hours. The reaction mixture was poured into ice water, and hydrochloric acid was added thereto. The mixture was extracted with dichloromethane-tetrahydrofuran (3:1), the extract was dried, and then the solvent was removed. The resulting crystals were washed with ethyl acetate and dried to obtain 580 mg of 2-(1,3-isoindolinedion-2-yl)-5-(3-carboxy-3,3-dimethylpropionyl)indane.
후처리
- temperaturerefluxed
- temperatureunder heating for 4 hours
- additionwas added
- extractionThe mixture was extracted with dichloromethane-tetrahydrofuran (3:1)
- customthe extract was dried
- customthe solvent was removed
- washThe resulting crystals were washed with ethyl acetate
- customdried
출처 및 근거
- ORD 기록
- ord-f44f7f3c34af49678323681509c06b5b
- 출처 데이터셋
- uspto-grants-1998_04
- 특허 번호
- US05739132
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