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氯米芬柠檬酸盐(1,Clomid)为抗不育症最常用药物之一,因其制备不易而价贵。本文报道其关键中间体2的一步简便有效合成新法。路线A 二苯乙炔的己烷溶液于0℃滴加二异丁基铝氢化物,室温反应1小时,55℃反应18小时,冷至室温备用。四(三苯基膦)钯(3)、4-[2-(二乙基氨基)乙氧基]溴苯(4)和THF混合,加入上述乙烯铝烷溶液,回流24小时,得2,收率60％。路线B 4、镁和THF回流,加入溴乙烷(二倍量稍多)反应3小时得格氏试剂,加
Clomiphene citrate (1, Clomid) is one of the most commonly used anti-infective drugs, because of its preparation is not easy and expensive. In this paper, we report a new simple and effective method for the synthesis of its key intermediate 2. Route A solution of diphenylacetylene in hexane at 0 ° C was added diisobutylaluminum hydride at room temperature for 1 hour, 55 ° C for 18 hours and cooled to room temperature for use. (Triphenylphosphine) palladium (3), 4- [2- (diethylamino) ethoxy] bromobenzene (4) and THF were mixed and the above vinylalne solution was added and refluxed for 24 hours to obtain 2, Yield 60%. Route B 4, magnesium and THF reflux, add bromoethane (twice more) for 3 hours to get Grignard reagent, plus