Synthesis and Crystal Structure of 2-Methoxy-benzoic Acid 2-Oxo-3-(2,4,6-trimethyl-phenyl)-1-oxa-spi

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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-methoxylben-zoyl chloride,and characterized by 1H 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 a = 10.6945(7),b = 12.8176(7),c = 16.4223(10) ,β = 103.5665(17)o,V = 2188.3(2) 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 ) bond is significantly shorter than the normal single C-C bond(1.53 ),suggesting that the carbonyl group on C(1) has formed a conjugated system with a double bond on C(2) and C(12). The new title compound 2-methoxy-benzoic acid 2-oxo-3- (2,4,6-trimethyl-phenyl) -1- oxa-spiro [4.4] non-3-en- ) has been synthesized by the condensation reaction of 4-hydroxy-3- (2,4,6-trimethyl-phenyl) -1 -oxa-spiro [4.4] methoxylbenzyl chloride, and characterized by 1H 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 a = 10.6945 (7), b = 12.8176 Β = 103.5665 (17) o, V = 2188.3 (2) 3, Z = 4, Dc = 1.234 g / cm3, F (000) = 864.000, μ = 0.085 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 ) bond is significantly shorter than the Normal single CC bond (1.53 ), suggesting that the carbonyl group on C (1) has formed an conjugated system with a double bond on C (2) and C (12).
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