3-氯-3-甲基-1-丁炔是重要的化工有机中间体,可用于农药、杀菌剂、除草剂等多种化工领域。制备方法:将1000 kg 3-甲基丁炔-3-醇投入到275 kg的36%盐酸中(氯化釜),加入氯化亚铜10kg,然后将1200 kg间苯二甲酸与1440 kg三氯甲基苯投入到酰氯化釜中并升温至70 ~85 ℃,投入1.5kg三氯化铁,保温3小时后滴加1440 kg三氯甲基苯,3小时滴加完毕。期间,冷媒设置温度为-20 ℃,盐酸洗涤塔中盐酸为外购浓盐酸,浓度为30%,洗涤过程洗涤液温度为40 ~ 45 ℃。盐酸洗涤液中回收的苯甲酸纯度为97.32%,最后得到的3-氯-3-甲基丁炔的纯度为94.57%,收率96.28%。
农药; 杀菌剂; 除草剂
合成路线 1(1. 合成:1111-97-3)
- 产率:95%
- 条件:With hydrogenchloride; sulfuric acid; zinc(II) chloride In water at 0 - 5℃; for 2 h;
- 步骤:打开氯化反应器并返回冷冻阀。将反应容器冷却至10℃,依次加入盐酸、氯化锌和聚乙二醇600;将3-羟基-3-甲基丁烯和硫酸滴加到反应容器中,加完后保持0至5℃反应2小时。反应完成后转移到洗涤釜中洗涤,搅拌静置,分离水层后转移到泵送釜,抽滤、干燥得到3-氯-3-甲基丁烯(产率95%,纯度99%)。
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合成路线 2(2. 合成:1111-97-3)
- 产率:未提供
- 条件:未提供
- 步骤:未提供
- 参考文献:[1] Journal of the American Chemical Society, 1951, vol. 73, p. 4013
合成路线 3(3. 合成:1111-97-3)
- 产率:未提供
- 条件:未提供
- 步骤:未提供
- 参考文献:[1] Journal of the American Chemical Society, 1960, vol. 82, p. 4094 - 4097