Diazoacetophenone → Phosphonic acid, (5-benzoyl-2,4-dihydro-3H-pyrazol-3-ylidene)bis-, tetraethyl ester

참여 물질

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Ethenylidene bisphosphonic acid tetraethyl ester (II, PREPARATION 1, 6.00 g) in ether (20 ml) is treated with solid 2-diazo-1-phenylethanone (2.92 g) and stirred at 22° for 20 hrs. The precipitate is collected and washed with ether to give the title compound. An analytical sample is obtained by recrystallization from methylene chloride/hexane, mp 133.5°-134°; MS (m/e) 446, 327, 309, 281, 271, 253, 243, 215, 175; IR (mineral oil mull) 3183, 1631, 1600, 1578, 1548, 1433, 1260, 1242, 1161, 1067, 1043, 1020, 1001, 995, 976 and 962 cm-1 ; NMR (CDCl3) 8.10, 7.50, 6.90, 4.27, 3.69 and 1.34 δ.

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