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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℃ |
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