公开(公告)号：US6156906A

公开(公告)日：2000-12-05

申请号：US374949

申请日：1999-08-16

申请人： Shunji Hyoda ,  Masaharu Kita ,  Hirotoshi Sawada ,  Shuichi Nemugaki ,  Takahiro Ueta ,  Kohki Satoh ,  Sumio Otsuka ,  Yoshitaka Miyawaki ,  Hiroshi Taniguchi

发明人： Shunji Hyoda ,  Masaharu Kita ,  Hirotoshi Sawada ,  Shuichi Nemugaki ,  Takahiro Ueta ,  Kohki Satoh ,  Sumio Otsuka ,  Yoshitaka Miyawaki ,  Hiroshi Taniguchi

IPC分类号： C07D257/04 ,  C07D403/04

CPC分类号： C07D257/04

摘要： A process for the preparation of a 5,5'-bi-1H-tetrazole diammonium salt by dropwisely adding the aqueous hydrogen peroxide to which a small amount of weakly acidic substance has been added, to a starting aqueous solution containing hydrogen cyanide or sodium cyanide or potassium cyanide, sodium azide and a catalytic amount of copper sulfate preferably at a low temperature to maintain the pH of the reaction solution over a range of from 5 to 6, heating the reaction solution to effect the oxidation and cyclization reaction, reacting the reaction product with ammonium chloride or an aqueous solution thereof, and recovering the formed ammonium salt in the form of sparingly soluble crystals. The desired product is obtained in a high yield and in a high purity from the starting materials which are cheaply available and are easy to handle through a decreased number of steps, i.e., through a one-pot reaction without requiring cumbersome after-treatment.

摘要翻译： 通过向含有氰化氢或氰化钠的起始水溶液中滴加加入少量弱酸性物质的过氧化氢水溶液来制备5,5'-双-1H-四唑二铵盐的方法 或氰化钾，叠氮化钠和催化量的硫酸铜，优选在低温下将反应溶液的pH维持在5至6的范围内，加热反应溶液进行氧化和环化反应，使反应 与氯化铵或其水溶液反应，并回收形成的微溶晶体形式的铵盐。 从廉价可得的起始原料以高产率和高纯度获得所需的产物，并且通过减少数量的步骤，即通过一锅反应而不需要繁琐的后处理容易处理。

公开(公告)号：US07122676B2

公开(公告)日：2006-10-17

申请号：US09813826

申请日：2001-03-22

申请人： Shunji Hyoda ,  Masaharu Kita ,  Hirotoshi Sawada ,  Shuichi Nemugaki ,  Takahiro Ueta ,  Kohki Satoh

发明人： Shunji Hyoda ,  Masaharu Kita ,  Hirotoshi Sawada ,  Shuichi Nemugaki ,  Takahiro Ueta ,  Kohki Satoh

IPC分类号： C07D257/04 ,  B01J19/00

CPC分类号： C07D257/04 ,  C07C257/22

摘要： A process for preparing 5,5′-bi-1H-tetrazolediammonium salts (BHT.2NH3) maintaining a high yield through oxaldiimidic acid dihydrazide (OAH) from the starting materials which are cheaply available and are easy to handle. The 5,5′-bi-1H-tetrazolediammonium salts (BHT.2NH3) are prepared by dissolving the oxaldiimidic acid dihydrazide (OAH) obtained by the reaction of hydrated hydrazide with dicyan in an aqueous solution of a weakly acidic compound such as acetic acid, dropwisely adding an aqueous solution of sodium nitrite thereto to form an azide thereof and to effect the cyclization reaction by heating, adding an aqueous solution of sodium hydroxide to the reaction product to convert it into a 5,5′-bi-1H-tetrazoledisodium salt (BHT.2Na), reacting it with an aqueous solution of ammonium chloride, and recovering the formed ammonium salt as sparingly soluble crystals.

摘要翻译： 通过草本二酰亚胺二酰肼（OAH）从起始原料中制备的5,5'-双-1,5-四唑基铵盐（BHT.2NH 3 N 3）的方法，该方法是廉价可得的并且容易 处理。 通过将通过水合酰肼与二氰反应得到的草二酰亚胺二酰肼（OAH）溶解在水溶液中，制备5,5'-双-1H-四唑基铵盐（BHT.2NH 3 N 3） 弱酸性化合物如乙酸，向其中逐滴加入亚硝酸钠水溶液形成叠氮化物，通过加热进行环化反应，向反应产物中加入氢氧化钠水溶液，将其转化为5， 5'-双-1,5-四唑基二钠盐（BHT.2Na），与氯化铵水溶液反应，回收形成的铵盐作为微溶晶体。

公开(公告)号：US06433181B1

公开(公告)日：2002-08-13

申请号：US09871946

申请日：2001-06-04

申请人： Shunji Hyoda ,  Masaharu Kita ,  Atsushi Sugino ,  Shuichi Nemugaki ,  Takahiro Ueta ,  Koki Sato

发明人： Shunji Hyoda ,  Masaharu Kita ,  Atsushi Sugino ,  Shuichi Nemugaki ,  Takahiro Ueta ,  Koki Sato

IPC分类号： C07D25704

CPC分类号： C07D257/04

摘要： A process for the preparation of a highly pure 5,5′-bi-1H-tetrazolediammonium salt comprising adding a small amount of ammonia water to a reaction solution containing a 5,5′-bi-1H-tetrazolediammonium salt synthesized in the presence of a copper catalyst, removing by filtration the blue insoluble components of formed copper.ammonia.5,5′-bi-1H-tetrazole complex to obtain a filtrate of the 5,5′-bi-1H-tetrazoledisodium salt and reacting the filtrate with an aqueous solution of ammonium chloride, and recovering the formed, highly pure ammonium salt as sparingly soluble crystals.

摘要翻译： 一种制备高纯度5,5'-双-1,5-四唑基铵盐的方法，包括向含有5,5'-双-1,5-四唑基铵盐的反应溶液中加入少量氨水，该反应溶液在 铜催化剂，通过过滤除去形成的铜五氢-5,5'-双-1,5-四唑络合物的蓝色不溶性组分，得到5,5'-双-1,5-四唑基二钠盐的滤液，并将滤液与 氯化铵水溶液，并回收形成的高纯度铵盐作为微溶晶体。