CN101693691A - 一种5-氨基-3-氰基-1-[(2,6-二氯-4-三氟甲基)苯基]-1氢-吡唑的制备方法 - Google Patents
一种5-氨基-3-氰基-1-[(2,6-二氯-4-三氟甲基)苯基]-1氢-吡唑的制备方法 Download PDFInfo
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实施例编号 | 氰基乙酸乙酯与2,6-二氯-4三氟甲基苯胺重氮盐的摩尔比 | 反应温度(℃) | 反应时间(小时) | 萃取用溶剂 | 收率(%) |
实施例4 | 1.1∶1 | 20 | 3 | 三氯甲烷 | 88 |
实施例5 | 1.3∶1 | 23 | 4 | 1,2-二氯乙烷 | 92 |
实施例6 | 1.4∶1 | 27 | 4 | 甲苯 | 86 |
实施例7 | 1.5∶1 | 30 | 5 | 苯 | 84 |
实施例编号 | 化合物(I)产率(%) | 化合物(I)纯度(%) | 总收率(%) |
实施例8 | 96 | 98.0 | 84.5 |
实施例9 | 96 | 98.1 | 88.3 |
实施例10 | 96 | 97.9 | 82.6 |
实施例11 | 96 | 97.8 | 80.6 |
实施例编号 | 氰化物 | 化合物II、氰化物与甲醛的摩尔比 | 溶解(II)所用溶剂 | 萃取用溶剂 | 氨水与(III)摩尔比 | pH | 环化反应温度(℃) | 环化反应时间(小时) | 产品收率(%) | 总收率(%) |
实施例12 | 氰化钾 | 1∶1∶1.1 | 甲醇 | 苯 | 1∶1 | 9 | 30 | 4 | 88 | 83.6 |
实施例13 | 氰化亚铜 | 1∶1∶1.1 | 乙醇 | 二甲苯 | 3∶1 | 10 | 32 | 5 | 93 | 88.4 |
实施例14 | 亚铁氰化钾 | 1∶1∶1.1 | 异丙醇 | 氯苯 | 4∶1 | 11 | 34 | 6 | 92 | 87.4 |
实施例15 | 氰化钠 | 1∶1∶1.2 | 环丁砜 | 甲苯 | 5∶1 | 9 | 36 | 7 | 90 | 85.5 |
实施例16 | 氰化钾 | 1∶1∶1.1 | THF | 苯 | 2∶1 | 9 | 38 | 8 | 85 | 80.8 |
实施例17 | 氰化亚铜 | 1∶1∶1.1 | NMP | 二甲苯 | 3∶1 | 9 | 40 | 3 | 82 | 77.9 |
实施例18 | 亚铁氰化钾 | 1∶1∶1.3 | DMF | 氯苯 | 4∶1 | 9 | 30 | 4 | 80 | 76.0 |
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CN2009102360960A CN101693691B (zh) | 2009-10-27 | 2009-10-27 | 一种5-氨基-3-氰基-1-[(2,6-二氯-4-三氟甲基)苯基]-1氢-吡唑的制备方法 |
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Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
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CN113372240A (zh) * | 2021-07-02 | 2021-09-10 | 湖北金玉兰医药科技有限公司 | 一种2,3-二氰基丙酸乙酯的绿色制备工艺 |
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Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
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CN113372240A (zh) * | 2021-07-02 | 2021-09-10 | 湖北金玉兰医药科技有限公司 | 一种2,3-二氰基丙酸乙酯的绿色制备工艺 |
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