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清风绰影木虫 (著名写手)
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 [ Last edited by 清风绰影 on 2010-10-21 at 10:20 ] |
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清风绰影(金币+88, 翻译EPI+1):非常感谢，辛苦了！ 2010-10-22 10:57:11
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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% |
2楼2010-10-22 09:44:02
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12.2g of the Nitron were decomposed with 120ml of 6N sulfuric acid in the presence of 240ml of ether, and stirred for 1 hour. The ether layer was separated, and the aqueous layer was extracted with ether several times. The combined ether layer was washed with water, dried, followed by distillation of the solvent. The residue oil was distilled at 74℃ at 16mmHg ( Claisen flask), yield 1.6g. As analysis indicates, it was Fumaric acid- monoaldehyde ethyl ester. (obviously formed through the ester change from the methyl ester in the formation of the Nitron) The Fumaric acid- monoaldehyde ethyl ester is liquid at room temperature and forms a insoluble, good crystalline 2,4-dinitrophenylhydrazone, m.p. 153℃ |
3楼2010-10-22 10:22:21
