Synthesis and Crystal Structure of 2-Methoxybenzoic Acid 2-Oxo-3-(2,4,6-trimethyl-phenyl)-1-oxa-spir

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T The new title compound 2-methoxy-benzoic acid 2-oxo-3-(2,4,6-trimethyl-phenyl)-1-oxa-spiro[4.4]non-3-en-4-yl ester(3,C25H26O5)has been synthesized by the condensation reaction of 4-hydroxy-3-(2,4,6-trimethyl-phenyl)-1-oxa-spiro[4.4]non-3-en-2-one(2)with 2-methoxylbenzoyl chloride,and characterized by 1 H NMR and MS spectra.Its crystal structure was determined by single-crystal X-ray diffraction.The crystal is of monoclinic,space group P21/c with α=10.6945(7),b=12.8176(7),c=16.4223(10)(A),β=103.5665(17)°,V=2188.3(2)(A)3,Z=4,Dc=1.234 g/cm3,F(000)=864.000,μ=0.085 mm-1,the final R=0.0520 and wR=0.1132 for 2732 observed reflections with Ⅰ>2σ(Ⅰ).In the crystal structure,the C(1)-C(2)(1.478(A))bond is significantly shorter than the normal single C-C bond(1.53 A),suggesting that the carbonyl group on C(1)has formed a conjugated system with a double bond on C(2)and C(12).
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