반응식
[C:1]1(=[O:11])[O:6][C:4](=[O:5])[C:3]2=[CH:7][CH:8]=[CH:9][CH:10]=[C:2]12.[Cl:12][C:13]1[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=1.[Cl-].[Al+3].[Cl-].[Cl-]>O>[Cl:12][C:13]1[CH:18]=[CH:17][C:16]([C:4]([C:3]2[CH:7]=[CH:8][CH:9]=[CH:10][C:2]=2[C:1]([OH:6])=[O:11])=[O:5])=[CH:15][CH:14]=1참가 물질
실험 절차
To a solution prepared by adding 30 g (0.2 mol.) of phthalic anhydride to 122 ml of dried chlorobenzene, was added 64 g (0.48 mol.) of well-ground anhydrous aluminium chloride with stirring. The reaction temperature rose gradually, and the reaction system reached a refluxing condition. The refluxing was continued for 1 hour as the reaction temperature was controlled so that the reaction system refluxed moderately using the ice bath. Then, the reaction product solidified spontaneously. 300 ml of water was added dropwise to the reaction system while cooling by means of an ice bath. The thus produced white precipitate was thoroughly washed with water and cooled ethanol to obtain 45 g of crude crystals. These crude crystals were recrystallized from benzene to obtain the intended compound. Yield 38 g, Melting Point 146° to 148° C.
후처리
- customTo a solution prepared
- temperaturerefluxed moderately
- temperaturewhile cooling by means of an ice bath
- washThe thus produced white precipitate was thoroughly washed with water
- temperaturecooled ethanol
출처 및 근거
- ORD 기록
- ord-32bc8f3a6462456696a6fbda4f1bf644
- 출처 데이터셋
- uspto-grants-1985_02
- 특허 번호
- US04500636
연결된 노트
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