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[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.C([NH2:16])CCC>ClCCl>[C:1]([O-:6])(=[O:11])[C:2]1[C:3](=[CH:7][CH:8]=[CH:9][CH:10]=1)[C:4]([NH2:16])=[O:5].[NH4+:16]참가 물질
실험 절차
A heterogenous mixture of phthalic anhydride (10.0 g, 67.5 mmol) and 100 mL of dichloromethane was cooled in an ice bath. n-Butyl amine (12.345 g, 168.78 mmol) was added dropwise. The temperature was not allowed to rise above 15° C. during the addition. When a small amount of the amine had been added a homogenous solution resulted. After a short time, a white precipitate formed. As more amine was added, the precipitate redissolved and a solution again formed. Upon completion of the addition the reaction was allowed to stir in an ice bath for 10 minutes. A white precipitate again formed. The mixture was allowed to stir at 0° C. for 50 minutes and at room temperature for 10 minutes. The precipitate was filtered off and washed with a small amount of dichloromethane. Washing with hexanes and drying in air afforded 8.86 g of compound AM-1. NMR was in agreement with the proposed structure.
후처리
- temperaturewas cooled in an ice bath
- additionto rise above 15° C. during the addition
- customresulted
- customAfter a short time, a white precipitate formed
- dissolutionthe precipitate redissolved
- customa solution again formed
- additionUpon completion of the addition the reaction
- customA white precipitate again formed
- stirringto stir at 0° C. for 50 minutes and at room temperature for 10 minutes
- filtrationThe precipitate was filtered off
- washwashed with a small amount of dichloromethane
- washWashing with hexanes
- customdrying in air
출처 및 근거
- ORD 기록
- ord-684655c60de84e89bb53f129a486d98c
- 출처 데이터셋
- uspto-grants-1996_08
- 특허 번호
- US05545505
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