反应详情

Diphenyl ether (20 ml) was heated to 260° C. or above, and a solution of 6.87 g of N-(3-oxo-1-cyclohexen-1-yl)aminomethylenemalonic acid diethyl ester in 5 ml of diphenyl ether was added thereto drop by drop. The resulting reaction mixture was refluxed for 15 minutes. After being allowed to cool, the reaction mixture was poured into 300 ml of n-hexane. The precipitate so formed was separated by filtration and then purified to obtain a yield of 4.37 g of the desired compound in the form of a pale-yellow powder. This compound melted (and decomposed) at 221°-224° C. Its infrared absorption spectrum (KBr tablet) had absorption peaks at 3340, 2960, 1740, 1690, 1635, 1605, 1560, 1510, 1285, 1170, 1150, 1090, 1035, 920 and 815 cm-1, and its n.m.r. spectrum (d6 -DMSO, 60Mc, TMS) had signals at δ values of 1.31 (3H, t, J=7 Hz), 1.9-3.1 (6H, m), 4.27 (2H, q, J=7 Hz), and 8.55 (1H, s).

1. customThe resulting reaction mixture
2. temperaturewas refluxed for 15 minutes
3. temperatureto cool
4. customThe precipitate so formed
5. customwas separated by filtration
6. custompurified