5-溴甲基-a,a,a',a'-四甲基-1,3-二乙氰基苯(阿那曲唑EP杂质C)是阿那曲唑的杂质(杂质D)。
医药
合成路线1
- 步骤: 将3,5-双(1-氰基-1-甲基乙基)甲苯(600g,2.65mol)、N-溴代琥珀酰亚胺(519g,2.916mol)、过氧化苯甲酰(17g,0.053mol)的混合物加入四氯化碳(4.5L)中,回流反应2-2.5小时;反应完成后冷却、过滤,滤液在40-45℃浓缩至干;所得固体在75-80℃下溶于2-丙醇(2L),缓慢冷却至10-15℃搅拌1小时,进一步冷却至-5-0℃搅拌2小时,过滤,用预冷2-丙醇(200ml)洗涤滤饼,再用正己烷洗涤吸干,最后40-45℃真空干燥,得到目标产物。
- 条件: 反应溶剂为四氯化碳,反应温度为回流(约76.8℃),后处理涉及2-丙醇溶解与分步冷却结晶、正己烷洗涤、真空干燥(40-45℃)。
- 收率: 87.0%(700.2g)
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