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发明公开
CN105037197A 偶氮二甲酸二-4-三氟甲基苄酯、中间体及其制备方法 无效 - 驳回

偶氮二甲酸二-4-三氟甲基苄酯、中间体及其制备方法
摘要：
本发明公开的新型偶氮试剂偶氮二甲酸二-4-三氟甲基苄酯、中间体及其制备方法，其制备方法依次包括以下步骤：以4-三氟甲基苄醇、三光气为原料，氯代烷烃为溶剂，在冰水浴下反应生成氯甲酸-4-三氟甲基苄酯，反应液经弱碱溶液洗涤后，室温下缓慢滴加一水合肼得到肼二甲酸二-4-三氟甲基苄酯；肼二甲酸二-4-三氟甲基苄酯再经氧化剂氧化得偶氮二甲酸二-4-三氟甲基苄酯。采用本发明制备偶氮二甲酸二-4-三氟甲基苄酯条件温和，步骤少，操作简单，收率高。
摘要（英）：

The invention discloses a novel azo-type reagent of di(4-trifluoromethylbenzyl) azodiformate, an intermediate, and a preparation method of di(4-trifluoromethylbenzyl) azodiformate. The preparation method comprises the following steps in sequence: taking 4-trifluoromethylbenzyl alcohol and triphosgene as raw materials and taking chloralkane as a solvent; performing reaction in an ice-water bath to produce 4-trifluoromethylbenzyl chloroformate; after washing the reacting liquid with a weakly alkaline solution, slowly adding hydrazine monohydrate drop by drop at a room temperature to obtain di(4-trifluoromethylbenzyl) hydrazinodiformate; and obtaining di(4-trifluoromethylbenzyl) azodiformate from di(4-trifluoromethylbenzyl) hydrazinodiformate through oxidation by an oxidizing agent. According to the invention, the preparation method of di(4-trifluoromethylbenzyl) azodiformate is mild in condition, less in step, simple in operation, and high in yield.

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