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本文简要地报道标题化合物8的新合成方法,并自8制备了4-脱甲氧基-7,9,13-三脱氧柔红酮11。以对二甲氧基苯1为起始原料,制得2,5-二甲氧基苯丁酮2,为淡黄色粘稠液体,bp 130～132°/2mm。(文献为橙色液体,bp 178°/3mm)。将2和溴反应可得α-溴代-2,5-二甲氧基苯丁酮 3,为淡黄色油状物,bp 157～160°/2mm。将3和丙二酸二乙酯钠反应,可得到双酯4,为白色结晶,mp34～34.5°。将4在DMSO-H_2O-NaCl介质中脱除乙氧羰基成单酯5,为淡黄色油状物,bp 232～234°。将5以钾硼氢还原,通过分子内的酯交换得到内酯6,为白
This article reports briefly on the new synthesis of the title compound 8 and 4-demethoxy-7,9,13-trideoxyfucolone 11 from 8. Starting from p-dimethoxybenzene 1, 2,5-dimethoxybutanone 2 was obtained as a pale yellow viscous liquid, bp 130-132 ° / 2 mm. (Literature is orange liquid, bp 178 ° / 3 mm). Reaction of 2 with bromine gave α-bromo-2,5-dimethoxybutanone 3 as a pale yellow oil, bp 157-160 ° / 2 mm. The 3 and diethyl malonate reaction of sodium, diester 4 can be obtained as white crystals, mp 34 ~ 34.5 °. The 4 in DMSO-H_2O-NaCl medium ethoxycarbonyl removal monoester 5, as a light yellow oil, bp 232 ~ 234 °. Reduction of 5 with potassium borohydride gave lactone 6 by intramolecular transesterification as white