반응식
[CH3:1][C:2]1[CH:7]=[C:6]([CH3:8])[N:5]=[C:4]([O:9][CH2:10][C:11]([O:13]CC)=[O:12])[N:3]=1.[OH-].[Na+]>C(O)C>[CH3:8][C:6]1[CH:7]=[C:2]([CH3:1])[N:3]=[C:4]([O:9][CH2:10][C:11]([OH:13])=[O:12])[N:5]=1참가 물질
4
실험 절차
2g (9.5mmol) of the ethyl ester prepared in Example 7 were dissolved in 20ml of ethanol. 25ml of an aqueous solution (10% by vol) of sodium hydroxide were then added to the solution. The reaction mixture was refluxed for 4 hours. After the reaction was complete, as confirmed by thin layer chromatography, the ethanol was evaporated off, the aqueous residue cooled, acidified to a pH of 2 and the product extracted into chloroform. Following drying first over anhydrous sodium sulphate and then by evaporation, 0.6g (yield 35% by weight) of a reddish oil were obtained which oil crystallised on standing.
후처리
- temperatureThe reaction mixture was refluxed for 4 hours
- customthe ethanol was evaporated off
- temperaturethe aqueous residue cooled
- extractionthe product extracted into chloroform
- dry with materialFollowing drying first over anhydrous sodium sulphate
- customby evaporation
출처 및 근거
- ORD 기록
- ord-c66387b1542d44ae88d0c2fcdcc585d9
- 출처 데이터셋
- uspto-grants-1992_08
- 특허 번호
- US05139563
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