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ChemicalBook CAS DataBase List Tolvaptan
150683-30-0

Tolvaptan synthesis

10synthesis methods
Tolvaptan is a selective, competitive vasopressin receptor 2 antagonist used to treat hyponatremia (low blood sodium levels) associated with congestive heart failure, cirrhosis, and the syndrome of inappropriate antidiuretic hormone (SIADH).
Synthetic Routes
  • ROUTE 1
  • 202112076457409268.jpg

    Cordero-Vargas, Alejandro; Quiclet-Sire, Beatrice; Zard, Samir Z. A flexible approach for the preparation of substituted benzazepines: Application to the synthesis of tolvaptan. Bioorganic & Medicinal Chemistry. Volume 14. Issue 18. Pages 6165-6173. 2006.

  • ROUTE 2
  • 202112073492714877.jpg

    Torisawa, Yasuhiro; Abe, Kaoru; Muguruma, Yasuaki; Fujita, Shigekazu; Ogawa, Hidenori; Utsumi, Naoto; Miyake, Masahiro. Process for preparation of benzoylaminobenzoylbenzazepinones by reaction of benzazepinones with benzoylaminophenyl halides in the presence of carbonylating agents. Assignee Otsuka Pharmaceutical Co., Ltd., Japan. WO 2007026971. (2007).

  • ROUTE 3
  • 202112075666521270.jpg

    Zard, Samir; Cordero Vargas, Alejandro; Sire, Beatrice. Improved process for the preparation of benzazepines and their derivatives. Assignee Centre National de la Recherche Scientifique CNRS, Fr.; Ecole Polytechnique. FR 2867187. (2005).

  • ROUTE 4
  • 202112075738626349.jpg

    Gao, Junlong; Li, Peng; Liu, Kai; Guo, Dapeng. Method for preparing high-purity Tolvaptan intermediate. Assignee Jiangsu Hengrui Medicine Co., Ltd., Peop. Rep. China. CN 108503586. (2018).

  • ROUTE 5
  • 202112072032224656.jpg

    Han, Shin; Jeon, Seong Hyeon; Lee, Shin Yoon. Improved method for preparing synthetic intermediates for tolvaptan. Assignee Hexa Pharmatec Co., Ltd., S. Korea. JP 2018012690. (2018).

  • ROUTE 6
  • 202112071752619277.jpg

    Guo, Xinfu; Wang, Qiang; Liu, Zhaoguo; Wang, Zhipeng. Preparation method of tolvaptan. Assignee Tianjin Taipu Pharmaceutical Co., Ltd., Peop. Rep. China. CN 106883175. (2017).

  • ROUTE 7
  • 202112071610528234.jpg

    Lixin, Juanzi; Li, Jianzhi; Ma, Xilai; Chi, Wangzhou; Liu, Hai; Hu, Xuhua; Zheng, Xiaoli; Zhai, Zhijun; Li, Jianxun. Process for the preparation of tolvaptan. Assignee Shanghai Tianci International Pharmaceutical Co., Ltd., Peop. Rep. China. CN 105753735. (2016).

  • ROUTE 8
  • 202112074808747122.jpg

    Patel, Dhaval J.; Shah, Tejas C.; Singh, Manoj Kumar. A process for the preparation of tolvaptan. Assignee Cadila Healthcare Limited, India. IN 2012MU01559. (2014).

  • ROUTE 9
  • 202112078492671377.jpg

    Sethi, Madhuresh Kumar; Rawat, Vijendrasingh; Thirunavukarasu, Jayaprakash; Yerramala, Raja Krishna; Kumar, Anish. Improved process for the preparation of tolvaptan. Assignee Matrix Laboratories Ltd., India. IN 2011CH01303. (2013).

  • ROUTE 10
  • 202112076434545671.jpg

    Chen, Tao; Chen, Hua; Yu, Lingli; Fan, Xiyuan. Method for preparing 2-carboxy-5-(2-methylbenzamido)toluene as Tolvaptan intermediate. Assignee Tianjin Taipu Medicine Science and Technology Development Co., Ltd., Peop. Rep. China. CN 103159641. (2013).

202112076457409268.jpg

Cordero-Vargas, Alejandro; Quiclet-Sire, Beatrice; Zard, Samir Z. A flexible approach for the preparation of substituted benzazepines: Application to the synthesis of tolvaptan. Bioorganic & Medicinal Chemistry. Volume 14. Issue 18. Pages 6165-6173. 2006.

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Yield:150683-30-0 96%

Reaction Conditions:

with methanol;sodium tetrahydroborate at 0; for 2 h;

Steps:

1.7 (7) Preparation of N-[4-[(7-chloro-2,3,4,5-tetrahydro-5-hydroxy-1H-1-benzazepine-1-yl)carbonyl]-3-methylphenyl]-2-methylbenzamide
7-chloro-5-hydroxy-2,3,4,5-tetrahydro-1H-1- benzazepine (19.0g, 42.51mmol) was dissolved in methanol (200ml) in a solvent, at 0 for Conditional batch of sodium borohydride (2.42g, 63.77mmol), after the addition was complete stirring was continued for 2h, TLC the reaction was complete. The reaction mixture was poured into water, extracted with methylene chloride, dried over anhydrous sodium sulfate, filtration and vacuum distillation of crude with methanol: petroleum ether (2: 1) and recrystallized to give a white solid tolvaptan (18.33g , 96.0%).

References:

Shanghai Tin Tsz Bio Valley Biological Engineering Co.;Li, Xinjuanzi;Li, Jianzhi;Ma, Xilai;Chi, Wangzhou;Liu, Hai;Hu, Xuhua;Zheng, Xiaoli;Di, Zhijun;Li, Jianxun CN105315169, 2016, A Location in patent:Paragraph 0170; 0211; 0212

FullText

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