|
|
清风绰影(金币+88, 翻译EPI+1):非常感谢，辛苦了！ 2010-10-22 10:57:11
Fumaric acid- monoaldehyde ethyl ester
7.0g γ-bromo crotonic acid methyl ester (I) were mixed with 20 ml of anhydrous pyridine with cooling. The reaction mixture became warm and turned red. Through addition of ether, the pyridinium salt II formed was precipitated and washed again with ether. Then it became an oil. After removal of ether, the obtained 9.85g of pyridinium salt was treated together with 5.8g of p-nitroso dimethyl aniline in 75 ml ethanol and 38.6 ml ?N. NaOH solution. The mixture became warm. After one hour it was diluted with water. After being kept in an ice tank for several hours, the Nitron III crystallized out. It was purified chromatographically using benzene through a 5cm-long aluminium oxide layer.
Calculated N 11.20% found N 11.42% |
|
回复此楼