methyl 2-[(11Z)-11-[3-(dimethylamino)propylidene]-6H-benzo[c][1]benzoxepin-2-yl]acetate | 113806-01-2

• 物质功能分类: 分析化学 - 标准品 - 药典标准品和杂质标准品
• 分子结构分类: 有机化合物 - 有机杂环化合物 - 苯并噁庚英
• 英文名称: methyl 2-[(11Z)-11-[3-(dimethylamino)propylidene]-6H-benzo[c][1]benzoxepin-2-yl]acetate
• CAS: 113806-01-2
• 化学式: C₂₂H₂₅NO₃
• 分子量: 351.4
• InChiKey: UGDFSHGFPJSALM-OCKHKDLRSA-N

物化性质

• 沸点：
  487.6±45.0 °C(Predicted)
• 密度：
  1.165±0.06 g/cm3(Predicted)

计算性质

• 辛醇/水分配系数(LogP)：
  4.1
• 重原子数：
  26
• 可旋转键数：
  6
• 环数：
  3.0
• sp3杂化的碳原子比例：
  0.32
• 拓扑面积：
  38.8
• 氢给体数：
  0
• 氢受体数：
  4

反应信息

• 作为产物：
  描述：

  盐酸奥洛他定 、 乙酰氯 、 碳酸氢钠 在 乙酸乙酯 、 Sodium sulfate-III 、 crude product 、 silica gel 、 methanol-dichloromethane 作用下， 以 甲醇 为溶剂， 反应 2.0h， 以to furnish {11-[3-Dimethylamino-prop-(Z)-ylidene]-6,11-dihydro-dibenz[b,e]oxepin-2-yl}-acetic acid methyl ester (0.22 g, 0.63 mmol) in 94% yield的产率得到methyl 2-[(11Z)-11-[3-(dimethylamino)propylidene]-6H-benzo[c][1]benzoxepin-2-yl]acetate
  参考文献：
  名称：

  Topical formulations for treating allergic diseases

  摘要：

  本发明揭示了使用三环化合物局部治疗眼、耳或鼻过敏疾病的方法。

  公开号：

  US20050288283A1

文献信息

• [EN] PROCESS FOR THE PREPARATION OF 11-[(Z)-3-(DIMETHYLAMINO)PROPYLIDENE]-6,11-DIHYDRO-DIBENZ[B,E]OXEPIN-2-YL]-ACETIC ACID<br/>[FR] PROCESSUS DE PREPARATION D'ACIDE 11-[(Z)-3-(DIMETHYLAMINO)PROPYLIDENE]-6,11-DIHYDRO-DIBENZ[B,E]OXEPIN-2-YL]-ACETIQUE
  申请人：URQUIMA SA

  公开号：WO2006010459A1

  公开（公告）日：2006-02-02

  Process for the preparation of olopatadine (I), which comprises reacting a compound of formula (V) in the presence of a palladium catalyst to provide a compound of formula (VI), wherein the acid protecting group is removed to provide the compound of formula (I) and if desired, transformation into its salts.

  制备奥洛帕坦丁（I）的过程包括在钯催化剂存在下，使式（V）化合物发生反应，得到式（VI）化合物，其中酸保护基被去除以得到式（I）化合物，并且如有需要，转化为其盐。
• Process for the preparation of (Z)-[11-(3-dimethylamino-propyliden)-6,11-dihydro-dibenzo[b,e]oxepin-2-yl]-acetic acid hydrochloride
  申请人：Urquima S.A.

  公开号：EP1908758A1

  公开（公告）日：2008-04-09

  The present invention relates an optimised process for the preparation of the compound of formula (Z)-[11-(3-dimethylamino-propyliden)-6,11-dihydro-dibenzo[b,e]oxepin-2-yl]-acetic acid hydrochloride in a higher purity, which comprises the preparation of salts of advanced intermediates and final crystallization of compound of formula 11-[(Z)-3-(dimethylamino)propylidene]-6,11-dihydro-dibenz[b,e]oxepin-2-yl]-acetic acid hydrochloride.

  本发明涉及一种优化的工艺，用于制备式(Z)-[11-(3-二甲基氨基丙烯基)-6,11-二氢二苯并[b,e]氧杂-2-基]-乙酸盐酸盐高纯度化合物，其包括先制备高级中间体的盐酸盐，再结晶式11-[(Z)-3-(二甲基氨基)丙烯基]-6,11-二氢二苯并[b,e]氧杂-2-基]-乙酸盐酸盐化合物。
• [EN] PROCESS FOR OBTAINING OLOPATADINE AND INTERMEDIATES<br/>[FR] PROCÉDÉ D'OBTENTION D'OLOPATADINE ET DE SES INTERMÉDIAIRES
  申请人：RAGACTIVES S L U

  公开号：WO2010007056A1

  公开（公告）日：2010-01-21

  Olopatadine can be obtained by means of a process comprising hydrolysis of a compound of general formula (II), wherein Y is OR1, wherein R1 is C1-C7 alkyl, C3-C7 cycloalkyl, aryl, arylalkyl, or heterocycle; or NR2R3, wherein R2 and R3, independently from each other, are C1-C7 alkyl, aryl, arylalkyl, or R2 and R3 together with the nitrogen atom to which they are bound form a heterocycle of 3 to 7 members, obtained by means of a process comprising reacting the corresponding ester or amide of 6,11-dihydro-11- oxodibenz[b,e]oxepin-2-acetic acid with a suitable Wittig reagent, in the presence of a base in a reaction medium comprising an organic solvent.

  Olopatadine可以通过一种过程获得，包括对通式（II）的化合物进行水解，其中Y为OR1，其中R1为C1-C7烷基，C3-C7环烷基，芳香族，芳香族烷基或杂环；或NR2R3，其中R2和R3独立地为C1-C7烷基，芳香族，芳香族烷基，或R2和R3与它们所结合的氮原子形成3至7个成员的杂环，通过在有机溶剂反应介质中，在碱存在下，与适当的Wittig试剂反应，获得6，11-二氢-11-氧代二苯[b，e]氧杂环-2-乙酸相应的酯或酰胺。
• PROCESS FOR OBTAINING OLOPATADINE AND INTERMEDIATES
  申请人：Silva Guisasola Luis Octavio

  公开号：US20120004426A1

  公开（公告）日：2012-01-05

  Olopatadine can be obtained by means of a process comprising hydrolysis of a compound of general formula (II), wherein Y is OR 1 , wherein R 1 is C 1 -C 7 alkyl, C 3 -C 7 cycloalkyl, aryl, arylalkyl, or heterocycle; or NR 2 R 3 , wherein R 2 and R 3 , independently from each other, are C 1 -C 7 alkyl, aryl, arylalkyl, or R 2 and R 3 together with the nitrogen atom to which they are bound form a heterocycle of 3 to 7 members, obtained by means of a process comprising reacting the corresponding ester or amide of 6,11-dihydro-11-oxodibenz[b,e]oxepin-2-acetic acid with a suitable Wittig reagent, in the presence of a base in a reaction medium comprising an organic solvent.

  Olopatadine可以通过以下过程获得：水解通式（II）的化合物，其中Y为OR1，其中R1为C1-C7烷基，C3-C7环烷基，芳基，芳基烷基或杂环；或者NR2R3，其中R2和R3分别独立地为C1-C7烷基，芳基，芳基烷基，或者R2和R3与它们所结合的氮原子形成3至7个成员的杂环，所述过程包括在有机溶剂的反应介质中，在碱的存在下，通过反应相应的6,11-二氢-11-氧代二苯[b，e]氧杂环-2-乙酸酯或酰胺与适当的Wittig试剂反应而得到。
• A PROCESS FOR THE SYNTHESIS OF OLOPATADINE
  申请人：COUNCIL OF SCIENTIFIC & INDUSTRIAL RESEARCH

  公开号：US20160280677A1

  公开（公告）日：2016-09-29

  The present invention provides a process for the synthesis of olopatadine. Further, the invention discloses a process that results in improved yield of the desired Z isomer.

  本发明提供了一种合成olopatadine的方法。此外，本发明揭示了一种能够提高所需Z异构体产量的方法。