化学合成
化学合成
合成路线 1(1. 合成:4619-20-9)
产率:99.3%
合成条件:at 50 - 60℃; for 2 h;
实验步骤:将75.7g琥珀酸酐溶于457.5ml甲苯中。分批加入220.5g无水AlCl3。 将反应混合物控制在50-60℃的温度。搅拌2小时后,通过TLC确认反应结束。 在剧烈搅拌下,将反应溶液缓慢滴加到1250ml 1mol / L冰盐酸中。逐渐沉淀出乳状固体,加完后,将混合物搅拌0.5小时并过滤。滤饼洗涤后 用甲苯和冰水,用50ml乙酸乙酯抽滤滤饼;缓慢加入溶液,加入500ml石油醚结晶。再搅拌0.5小时后,过滤,在40℃下干燥2小时,得到化合物 II144g。产率99.3%。[化合物II中间体]白色固体,
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