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1. 发明授权

US4388243A Process for the preparation of active-type vitamin D.sub.3 compounds 失效
标题翻译：活性型维生素D3化合物的制备方法
公开(公告)号：US4388243A
公开(公告)日：1983-06-14
申请号：US371870
申请日：1982-04-26
申请人： Osamu Nishikawa , Kenji Ishimaru , Toru Takeshita , Hideki Tsuruta
发明人： Osamu Nishikawa , Kenji Ishimaru , Toru Takeshita , Hideki Tsuruta
IPC分类号： C07J9/00
CPC分类号： C07J9/00 , Y02P20/55 , Y02P20/582
摘要： The present invention relates to a novel process for the preparation of active-type vitamin D.sub.3 compounds and their intermediates. In accordance with the present invention, a large amount of an active-type vitamin D.sub.3 compounds, for example 1.alpha.-hydroxycholecalciferol, 1.alpha.,25-dihydroxycholecalciferol and the like, is efficiently prepared with high industrial advantages by a novel processes, which comprises (i) reacting hydroxycholesta-5-enes having the hydroxyl groups protected with lower alkoxycarbonyl group as a starting material with allylic brominating agent and dehydrobrominating agent to prepare the corresponding hydroxycholesta-5,7-dienes, (ii) exposing the hydroxycholesta-5,7-dienes to ultraviolet irradiation or to a combination of the irradiation with thermal isomerization to obtain a mixture of the unreacted hydroxycholesta-5,7-dienes and previtamin D.sub.3 compounds or a mixture of the unreacted hydroxycholesta-5,7-dienes and the protected active-type vitamin D.sub.3 compounds, (iii) separating the mixture into the unreacted hydroxycholesta-5,7-dienes and previtamin D.sub.3 compounds or the protected active-type vitamin D.sub.3 compounds, (iv) recycling the unreacted hydroxycholesta-5,7-dienes as reuse and (v) thermally isomerizing the remaining compounds and/or splitting off the protective groups. The process for the preparation of active-type vitamin D.sub.3 compounds, in the present invention, is of very high industrial value, capable of carrying out by simple operation and adaptable to large scale commercial production.
摘要翻译：本发明涉及一种制备活性型维生素D3化合物及其中间体的新方法。根据本发明，通过新工艺有效地制备了大量活性型维生素D3化合物，例如1α-羟基胆钙化甾醇，1α，25-二羟基胆钙化甾醇等，具有高工业优势，其包括（i）使具有被低级烷氧基羰基保护的羟基作为起始原料的羟基胆甾-5-烯与烯丙基溴化剂和脱溴溴化剂反应以制备相应的羟基胆甾-5,7-二烯，（ii）将羟基胆甾-5， 7-二烯对紫外线照射或通过热异构化的照射的组合，得到未反应的羟基胆甾-5,7-二烯和维生素D3化合物的混合物或未反应的羟基胆甾-5,7-二烯与受保护的活性型维生素D3化合物，（iii）将混合物分离成未反应的羟基胆甾-5,7-二烯和维生素D3化合物或受保护的活性（iv）将未反应的羟基胆甾-5,7-二烯再循环使用，和（v）使其余化合物热异构化和/或分离保护基团。在本发明中制备活性型维生素D3化合物的方法具有非常高的工业价值，能够通过简单的操作进行并适应于大规模的商业生产。

2. 发明授权

US4298537A Process for producing steroid compounds having an oxo group in the side chain 失效
标题翻译：在侧链中具有氧代基的类固醇化合物的制备方法
公开(公告)号：US4298537A
公开(公告)日：1981-11-03
申请号：US97980
申请日：1979-11-28
申请人： Osamu Nishikawa , Kenji Ishimaru , Toru Takeshita , Hideki Tsuruta
发明人： Osamu Nishikawa , Kenji Ishimaru , Toru Takeshita , Hideki Tsuruta
IPC分类号： C07J9/00 , C07J53/00
CPC分类号： C07J9/005 , C07J9/00 , Y02P20/55
摘要： A process for producing a steroid compound having an oxo group in the side chain, which comprises condensing an acid halide having a steroid skeleton with an organozinc compound at the halocarbonyl group of the acid halide in an inert organic medium in the presence of a catalytic amount of an ether capable of forming a complex with the organozinc compound, and if desired, hydrolyzing the product. The process produces the steroid compound at a high yield, and often at an almost quantitative yield. The steroid compound is an important intermediate for the production of vitamin D.sub.3 analogs such as active forms of vitamin D.sub.3. In one preferred embodiment, an industrially advantageous process from the standpoint of operation is provided.
摘要翻译：一种制备侧链中具有氧代基的类固醇化合物的方法，该方法包括在惰性有机介质中，在催化量存在下将具有类固醇骨架的酰卤与有机锌化合物在酰卤的卤代羰基的能够与有机锌化合物形成络合物的醚，如果需要，水解产物。该方法以高产率产生类固醇化合物，并且通常以几乎定量的产率。类固醇化合物是生产维生素D3类似物（如活性形式的维生素D3）的重要中间体。在一个优选实施例中，提供了从工作角度出发的工业上有利的工艺。

3. 发明授权

US4292249A 25-Hydroxy-24-oxocholestane derivatives and preparation thereof 失效
标题翻译： 25-羟基-24-氧代胆乙醇衍生物及其制备
公开(公告)号：US4292249A
公开(公告)日：1981-09-29
申请号：US121857
申请日：1980-02-15
申请人： Osamu Nishikawa , Kenji Ishimaru , Toru Takeshita , Hideki Tsuruta
发明人： Osamu Nishikawa , Kenji Ishimaru , Toru Takeshita , Hideki Tsuruta
IPC分类号： C07J9/00 , C07J17/00
CPC分类号： C07J17/00 , C07J9/00
摘要： This invention relates to novel 25-hydroxy-24-oxocholestane derivatives and a process for preparing them.The novel 25-hydroxy-24-oxocholestane derivatives of this invention can easily be converted to 24,25-dihydroxycholecalciferol or 1.alpha.,24,25-trihydroxycholecalciferol which is known as useful for medicine controlling the calcium metabolism of warm-blooded animals. Moreover, 25-hydroxy-24-oxocholestane derivatives can be converted to novel 25-hydroxy-24-oxocholecalciferol expressed by the following formula ##STR1## and novel 1.alpha.,25-dihydroxy-24-oxocholecalciferol of the formula ##STR2## which are useful for medicine. The new 25-hydroxy-24-oxocholestane derivatives in the present invention are very useful as the intermediates for the synthesis of a variety of active vitamin D.sub.3.
摘要翻译：本发明涉及新的25-羟基-24-氧代胆乙醇衍生物及其制备方法。本发明的新型25-羟基-24-氧代胆乙醇衍生物可以容易地转化为24,25-二羟基胆钙化甾醇或1α，24,25-三羟基胆钙化甾醇，其已知可用于控制温血动物钙代谢的药物。此外，可以将25-羟基-24-氧代胆乙醇衍生物转化为由下式表示的新型25-羟基-24-氧代胆钙化甾醇和式（IMAGE）的新型1α，25-二羟基-24-氧代胆钙化甾醇，其为有用的药物。本发明中的新的25-羟基-24-氧代胆乙醇衍生物作为合成各种活性维生素D3的中间体是非常有用的。

4. 发明授权

US4153630A Inclusion compounds, process for preparation thereof, and process for separating isomers using the inclusion compounds 失效
标题翻译：包含化合物，其制备方法和使用包合物分离异构体的方法
公开(公告)号：US4153630A
公开(公告)日：1979-05-08
申请号：US735549
申请日：1976-10-26
申请人： Yataro Ichikawa , Yoshiyuki Yamanaka , Hideki Tsuruta , Mamoru Yamamoto , Kenichi Kato
发明人： Yataro Ichikawa , Yoshiyuki Yamanaka , Hideki Tsuruta , Mamoru Yamamoto , Kenichi Kato
IPC分类号： C07C7/152 , C07C13/70 , C07C15/02 , C07C37/86 , C07C39/06 , C07C39/07 , C07C39/28 , C07C41/34 , C07C201/16 , C07C7/00
CPC分类号： C07C201/16 , C07C13/70 , C07C15/02 , C07C37/86 , C07C41/34 , C07C41/44 , C07C67/60 , C07C7/152
摘要： An inclusion compound comprising meta-cyclophane of the formula ##STR1## and at least one benzene derivative included therein. And a process for separating an isomer containing a substituent at least at the 1- and 4-positions from a mixture containing isomers of a benzene derivative, which comprises contacting the meta-cyclophane with the mixture containing isomers of a benzene derivative thereby to form an inclusion compound in which an isomer containing a substituent at least at the 1- and 4-positions is included in the meta-cyclophane, then separating the inclusion compound from the mixture, and thereafter separating the isomer from the inclusion compound.
摘要翻译：包含式IMA IMA的间 - 环烷烃和包含其中的至少一种苯衍生物的包合物。以及至少在1位和4位含有取代基的异构体与含有苯衍生物异构体的混合物分离的方法，该方法包括使间 - 环烷烃与含有苯衍生物异构体的混合物接触，从而形成包含化合物，其中含有至少在1位和4位的取代基的异构体包括在间 - 环烷烃中，然后从混合物中分离包合物，然后将该异构体与包合物分离。

5. 发明授权

US4116955A Inclusion complex compound, process for its production, and method for its use 失效
标题翻译：包含复合化合物，其生产方法及其使用方法
公开(公告)号：US4116955A
公开(公告)日：1978-09-26
申请号：US802022
申请日：1977-05-31
申请人： Yataro Ichikawa , Mamoru Yamamoto , Hideki Tsuruta , Kenichi Kato , Teizo Yamaji , Eishin Yoshisato , Toshiyuki Hiramatsu
发明人： Yataro Ichikawa , Mamoru Yamamoto , Hideki Tsuruta , Kenichi Kato , Teizo Yamaji , Eishin Yoshisato , Toshiyuki Hiramatsu
IPC分类号： C07C69/587 , C07B31/00 , C07B63/02 , C07C1/00 , C07C2/00 , C07C7/00 , C07C7/152 , C07C11/00 , C07C11/02 , C07C13/70 , C07C27/00 , C07C33/02 , C07C45/00 , C07C45/85 , C07C47/21 , C07C49/203 , C07C51/00 , C07C51/487 , C07C57/02 , C07C57/03 , C07C67/00 , C07C107/00 , C09B27/00 , C09F5/00 , C11C1/00
CPC分类号： C07C49/203 , C07C13/70 , C07C45/85 , C07C47/21 , C07C51/487 , C07C67/60 , C07C7/152
摘要： An inclusion complex compound comprising (a) meta-cyclophane and (b) a trans-terpenoid of the formula ##STR1## wherein n is an integer of 1 to 9; A.sub.1 and A.sub.2 each represent (1) a hydrogen atom, (2) a halogen atom, (3) an inorganic group containing an oxygen, nitrogen or sulfur atom, (4) an organic group containing 1 to 5 carbon atoms, or (5) an organic group containing an oxygen, nitrogen or sulfur atom and 1 to 5 carbon atoms; and C* is the carbon atom of a carbonyl or methylene group,Included by the meta-cyclophane. This inclusion complex compound can be prepared by contacting the meta-cyclophane with a mixture containing the trans-terpenoid. A trans-terpenoid can be separated from a mixture containing it by utilizing an inclusion complex compound of it with meta-cyclophane.

6. 发明授权

US4456553A Vitamin D.sub.3 derivatives, process for preparation thereof, and antigens comprising said derivatives to be used for preparation of antibodies for immunochemical assay and antibodies prepared therefrom 失效
标题翻译：维生素D3衍生物，其制备方法和包含用于制备用于免疫化学测定的抗体的所述衍生物的抗原和由其制备的抗体
公开(公告)号：US4456553A
公开(公告)日：1984-06-26
申请号：US495877
申请日：1983-05-18
申请人： Jun-ichi Oshida , Osamu Nishikawa , Hideki Tsuruta , Toru Takeshita , Itaru Yamamoto , Kenji Ishimaru
发明人： Jun-ichi Oshida , Osamu Nishikawa , Hideki Tsuruta , Toru Takeshita , Itaru Yamamoto , Kenji Ishimaru
IPC分类号： C07J9/00
CPC分类号： C07J9/00 , Y10S530/807
摘要： The present invention relates to novel vitamin D.sub.3 derivatives which have a carboxyl group or its ester group at the 22-position, processes for the preparation thereof, and antigens, which comprise said vitamin D.sub.3 derivative and an immunogenic carrier material, to be used for the preparation of antibodies for enzymeimmunoassay or radioimmunoassay and antibodies obtained therefrom.The determination of such activated vitamin D.sub.3 compounds as 25-hydroxy vitamin D.sub.3, 24, 25-dihydroxy vitamin D.sub.3, etc. can be made satisfactorily according to the present invention.
摘要翻译：本发明涉及在22位具有羧基或其酯基的新型维生素D3衍生物，其制备方法，以及包含所述维生素D3衍生物和免疫原性载体材料的抗原，其用于制备用于酶免疫测定或放射免疫测定的抗体及其获得的抗体。根据本发明，可以令人满意地确定这种活化的维生素D3化合物作为25-羟基维生素D3,24,25-二羟基维生素D3等。

7. 发明授权

US3975441A Process for recovering purified 4-hydroxy-2,4,6-trimethyl-2,5-cyclohexadiene-1-one 失效
标题翻译：回收纯化的4-羟基-2,4,6-三甲基-2,5-环己二烯-1-酮的方法
公开(公告)号：US3975441A
公开(公告)日：1976-08-17
申请号：US464950
申请日：1974-04-29
申请人： Yataro Ichikawa , Yoshiyuki Yamanaka , Nobuo Suzuki , Hideki Tsuruta
发明人： Yataro Ichikawa , Yoshiyuki Yamanaka , Nobuo Suzuki , Hideki Tsuruta
IPC分类号： C07C49/713 , C07C45/00 , C07C45/29 , C07C45/39 , C07C45/51 , C07C45/80 , C07C45/82 , C07C67/00 , C07C45/24 , C07C29/26
CPC分类号： C07C45/80 , C07C45/29 , C07C45/39 , C07C45/516 , C07C45/82
摘要： A process for recovering purified 4-hydroxy-2,4,6-trimethyl-2,5-cyclohexadiene-1-one by distilling crude 4-hydroxy-,2,4,6-trimethyl-2,5-cyclohexadien-1-one. Preferably, the distillation is performed at a temperature of 40.degree. to 250.degree.C. using crude 4-hydroxy-2,4,6-trimethyl-2,5-cyclohexadien-1-one having a pH of 4 to 11.5. Thus, 4-hydroxy-2,4,6-trimethyl-2,5-cyclohexadien-1-one of high purity and reduced coloration can be recovered at a high recovery ratio.
摘要翻译：通过蒸馏粗4-羟基 - ，2,4,6-三甲基-2,5-环己二烯-1-酮来回收纯化的4-羟基-2,4,6-三甲基-2,5-环己二烯-1-酮的方法，一。优选地，使用pH为4至11.5的粗4-羟基-2,4,6-三甲基-2,5-环己二烯-1-酮，在40至250℃的温度下进行蒸馏。因此，可以高回收率回收高纯度和还原着色的4-羟基-2,4,6-三甲基-2,5-环己二烯-1-酮。

8. 发明授权

US4138553A 3-Methylene cephalosporanic acid derivatives and process for preparation thereof 失效
标题翻译： 3-亚甲基头孢菌酸衍生物及其制备方法
公开(公告)号：US4138553A
公开(公告)日：1979-02-06
申请号：US841321
申请日：1977-10-11
申请人： Sachio Ishimoto , Hisao Yamaguchi , Yoshinori Kato , Takeo Oba , Kenji Ozawa , Yataro Ichikawa , Koji Nakagawa , Hideki Tsuruta
发明人： Sachio Ishimoto , Hisao Yamaguchi , Yoshinori Kato , Takeo Oba , Kenji Ozawa , Yataro Ichikawa , Koji Nakagawa , Hideki Tsuruta
IPC分类号： C07D499/00 , C07D501/10 , C07D501/02
CPC分类号： C07D499/00 , Y02P20/55
摘要： Novel substituted hydrazide derivatives of 7-(substituted)amino-3-methylene-cepham-4-carboxylic acids expressed by the formula ##STR1## wherein R.sub.1 represents alkyl containing at least 3 carbon atoms, cycloalkyl, or optionally substituted aryl, and one of R.sub.2 and R.sub.3 represents hydrogen with the other being hydrogen or the same as R.sub.1 ; or R.sub.1 and R.sub.2 form a heterocyclic ring optionally through a hetero atom together with the attached nitrogen and R.sub.3 represents hydrogen atom; and Z.sub.1 represents amino or protected amino; and acid addition salts thereof, which are useful as intermediates for synthesizing cephalosporin antibiotics. These compounds can be prepared in high yields from the corresponding substituted hydrazide derivatives of 6-substituted amino-1-oxide-2, 2-dimethyl-penam-3-carboxylic acids, which are readily available at low costs, by heating them in the presence of a thermal rearrangement promotor such as organic sulfonic acids and optionally in the further presence of a tertiary nitrogen-containing cyclic compound, followed if desired by splitting off the amino-protecting group and converting the product to acid addition salts.
摘要翻译：由式“IMAGE”表示的7-（取代的）氨基-3-亚甲基 - 头孢烯-4-羧酸的新型取代的酰肼衍生物，其中R 1表示含有至少3个碳原子的烷基，环烷基或任选取代的芳基， R2和R3代表氢，另一个是氢或与R1相同; 或R 1和R 2与所连接的氮一起任选地通过杂原子形成杂环，并且R 3表示氢原子; Z1表示氨基或被保护的氨基; 其酸加成盐，其可用作合成头孢菌素抗生素的中间体。这些化合物可以以相当于6-取代的氨基-1-氧化物-2,2-二甲基 - 对甲苯磺酸的取代的酰肼衍生物的高收率制备，它们以低成本容易获得，通过在存在热重排促进剂如有机磺酸，并且任选地在另外存在叔氮气环状化合物的情况下，如果需要的话，分解氨基保护基并将产物转化成酸加成盐。

9. 发明授权

US3966818A Novel process for preparation of 4-hydroxy-2,4,6-trimethyl-2,5-cyclohexadiene-1-one 失效
标题翻译：用于制备4-羟基-2,4,6-三甲基-2,5-环己二烯-1-酮的新方法
公开(公告)号：US3966818A
公开(公告)日：1976-06-29
申请号：US342500
申请日：1973-03-19
申请人： Yataro Ichikawa , Yoshiyuki Yamanaka , Hideki Tsuruta
发明人： Yataro Ichikawa , Yoshiyuki Yamanaka , Hideki Tsuruta
IPC分类号： B01J31/22 , C07C45/39 , C07C45/16
CPC分类号： B01J31/2243 , B01J31/181 , B01J31/183 , B01J31/2234 , B01J31/26 , C07C45/39 , B01J2231/70 , B01J2531/025 , B01J2531/0252 , B01J2531/845
摘要： A process for preparing 4-hydroxy-2,4,6-trimethyl-2,5-cyclohexadiene-1-one comprising reacting 2,4,6-trimethyl phenol with molecular oxygen or a molecular oxygen-containing gas. The product (also called mesitylquinol) is an intermediate useful as a raw material for the synthesis of a variety of industrial chemicals such as a drugs, dyestuffs, and pigments.
摘要翻译：制备4-羟基-2,4,6-三甲基-2,5-环己二烯-1-酮的方法包括使2,4,6-三甲基苯酚与分子氧或含分子氧的气体反应。该产品（也称为均三甲基吗啉）是可用作合成各种工业化学品如药物，染料和颜料的原料的中间体。

10. 发明授权

US3957887A Process for preparing trimethylhydroquinone 失效
标题翻译：制备三甲基氯化铵的方法
公开(公告)号：US3957887A
公开(公告)日：1976-05-18
申请号：US391667
申请日：1973-08-27
申请人： Yataro Ichikawa , Yoshiyuki Yamanaka , Hideki Tsuruta
发明人： Yataro Ichikawa , Yoshiyuki Yamanaka , Hideki Tsuruta
IPC分类号： C07C27/00 , C07C37/07 , C07C39/08 , C07C67/00 , C07C37/00
CPC分类号： C07C37/07
摘要： This invention is directed to a process for preparing trimethylhydroquinone (TMHQ) by heating 4-hydroxy-2,4,6-trimethyl-2,5-cyclohexadiene-1-one (HTCD) in a nonacidic liquid medium consisting of either methanol or an aqueous medium, preferably in the presence of a basic substance, at a temperature of at least 100.degree.C., and preferably 150.degree.-300.degree.C.Thus, according to this invention, TMHQ of high purity and small coloration can be prepared from HTCD in good yield, for example, as high as 85 - 98%.

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